KWAME NKRUMAH UNIVERSITY OF SCIENCE AND

TECHNOLOGY

COLLEGE OF ENGINEERING

DEPARTMENT OF PETROLEUM ENGINEERING

LAB MANUAL FOR BSc. PETROLEUM ENGINEERING

(PETE 355)

1
PREFACE
This laboratory manual is designed for the course PETE 355 – Petroleum Engineering
Laboratory I to serve the following:

1) Provide students with knowledge about the basic laboratory equipment and
procedures used in core analysis and the theoretical aspects of the parameters.
2) Detailed description of laboratory exercises suitable for student work.
3) Knowledge of petrophysical and hydrodynamic properties of reservoir rocks.
4) Give the students some details about the analysis of cores and review the nature and
quality of the information that can be deduced from cores.
5) Knowledge of the physical properties of reservoir fluids and their practical application
in conducting a field study. These fluid properties are usually determined by
laboratory experiments performed on samples of actual reservoir fluids.

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Contents
PREFACE .................................................................................................................................................... 2
1. LABORATORY SAFETY ......................................................................................................................... 8
1.1. FIVE PRINCIPLES OF SAFETY ........................................................................................................ 8
1.3.1 PRACTICE SAFETY ............................................................................................................ 8
1.3.2 SAFETY OF OTHERS.......................................................................................................... 8
1.3.3 HAZARDS ASSOCIATED WITH YOUR PARTICULAR EXPERIMENT ................................. 8
1.3.4 WHAT TO DO IN AN EMERGENCY .................................................................................... 8
1.3.5 REPORT HAZARDS OR HAZARDOUS CONDITIONS.......................................................... 9
1.2. FIRST AID.................................................................................................................................... 9
1.3.6 STOPPAGE OF BREATHING .............................................................................................. 9
1.3.7 SEVERE BLEEDING ........................................................................................................... 9
1.3.8 THERMAL BURNS ............................................................................................................. 9
1.3.9 TRAUMATIC SHOCK ............................................................................................................ 9
1.3. SAFETY RULES ............................................................................................................................ 9
1.3.10 PERSONAL PRECAUTIONS ................................................................................................... 9
1.3.11 LABORATORY PRACTICE .................................................................................................... 10
1.4. CHEMICAL HAZARDS AND SAFETY PROCEDURES ...................................................................... 10
1.5. UNATTENDED CHEMICAL REACTIONS ....................................................................................... 10
1.6. TOXIC HAZARDS ....................................................................................................................... 11
1.7. ORGANIC SOLVENTS ................................................................................................................. 11
1.8. CHEMICAL WASTE DISPOSAL .................................................................................................... 11
1.9. ELECTRICAL HAZARDS AND SAFETY PROCEDURES..................................................................... 11
1.10. PRECAUTIONS ...................................................................................................................... 11
1.11. STATIC ELECTRICITY AND SPARK HAZARDS............................................................................ 12
2. INTRODUCTION ............................................................................................................................... 13
3. ROCK SAMPLE PREPARATION........................................................................................................... 16
3.1. CLEANING AND SATURATION DETERMINATION ........................................................................... 16
3.2. OBJECTIVES .............................................................................................................................. 16
3.3. INTRODUCTION AND THEORY ...................................................................................................... 16
3.4. LABORATORY METHODS .............................................................................................................. 16
3.5. DIRECT INJECTION OF SOLVENT ................................................................................................ 16
3.5.1. CENTRIFUGE FLUSHING ........................................................................................................ 16
3.5.2. GAS DRIVEN SOLVENT EXTRACTION...................................................................................... 16

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 3.5.3. SOXHLET EXTRACTION .......................................................................................................... 16
3.5.4. DEAN-STARK DISTILLATION-EXTRACTION.............................................................................. 16
3.5.5. VACUUM DISTILLATION ........................................................................................................ 17
3.6. SUMMARY ................................................................................................................................... 18
3.7. SATURATION DETERMINATION .................................................................................................... 18
3.7.1. DEFINITIONS......................................................................................................................... 18
3.8. SATURATION DETERMINATION, DEAN-STARK DISTILLATION METHOD (EXPERIMENT 1) ............... 19
3.8.1. DESCRIPTION........................................................................................................................ 19
3.8.2. PROCEDURE ......................................................................................................................... 19
3.8.3. DATA AND CALCULATIONS: .................................................................................................. 20
4. POROSITY ........................................................................................................................................ 21
4.1. DEFINITIONS ................................................................................................................................ 21
4.2. EFFECT OF COMPACTION ON POROSITY ....................................................................................... 22
4.3. POROSITY MEASUREMENTS ON CORE PLUGS ............................................................................... 22
4.4. BULK VOLUME MEASUREMENT................................................................................................ 22
4.5. PORE VOLUME MEASUREMENT ............................................................................................... 23
4.6. GRAIN VOLUME MEASUREMENT.............................................................................................. 25
4.7. EFFECTIVE POROSITY DETERMINATION BY HELIUM POROSIMETER METHOD (EXPERIMENT 2) . 25
4.7.1. DESCRIPTIONS ...................................................................................................................... 25
4.7.2. PROCEDURE ......................................................................................................................... 25
4.7.3. CALCULATIONS AND REPORT................................................................................................ 25
4.8. POROSITY DETERMINATION BY LIQUID SATURATING METHOD (EXPERIMENT 3) ...................... 26
4.8.1. DESCRIPTION........................................................................................................................ 26
4.8.2. PROCEDURE ......................................................................................................................... 26
4.8.3. CALCULATIONS AND REPORT:............................................................................................... 26
5. PERMEABILITY ................................................................................................................................. 27
5.1. DEFINITION .............................................................................................................................. 27
5.2. DARCY’S LAW ........................................................................................................................... 27
5.3. KLINKENBERG EFFECT............................................................................................................... 27
5.4. IDEAL GAS FLOW ...................................................................................................................... 28
5.5. HIGH VELOCITY FLOW .............................................................................................................. 29
5.6. MEASUREMENT OF PERMEABILITY ........................................................................................... 30
5.6.1. CONSTANT HEAD PERMEAMETER......................................................................................... 30
5.7. MEASUREMENT OF AIR PERMEABILITY (EXPERIMENT 4) .......................................................... 31
5.7.1. DESCRIPTION........................................................................................................................ 31
5.7.2. PROCEDURE ......................................................................................................................... 31
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 5.7.3. RESULTS AND CALCULATION: ............................................................................................... 32
5.8. ABSOLUTE PERMEABILITY MEASUREMENT OF WATER (EXPERIMENT 5) ................................... 32
5.8.1. DESCRIPTION........................................................................................................................ 32
5.8.2. PROCEDURE ......................................................................................................................... 32
5.8.3. CALCULATIONS AND REPORT................................................................................................ 32
5.8.4. CALCULATION OF KABS........................................................................................................... 33
6. DETERMINING DENSITY USING THE PYCNOMETER ........................................................................... 35
6.1. DENSITY ................................................................................................................................... 35
6.2. PRECAUTIONS .......................................................................................................................... 36
6.3. PYCNOMETRIC METHOD .......................................................................................................... 36
7. MEASURING THE SURFACE TENSION AND INTERFACIAL USING THE DU NOUY RING ........................ 38
7.1. PRE LAB ACTIVITY ..................................................................................................................... 38
7.2. MEASURING THE INTERFACIAL TENSION WITH THE DU NOUY RING. ........................................ 39
7.3. PRE LAB ACTIVITY ..................................................................................................................... 39
8. DETERMINATION OF VISCOSITY USING THE ROTATIONAL VISCOMETER (FANN M35SA) ................... 40
8.1. VISCOSITY TEST ........................................................................................................................ 40
8.2. MEASURING GEL STRENGTH..................................................................................................... 41
8.3. NEWTONIAN VISCOSITY CALCULATIONS ................................................................................... 42
9. DETERMINATION OF SPECIFIC GRAVITY USING API HYDROMETER METHOD .................................... 45
9.1. PROCEDURE; ............................................................................................................................ 45
9.2. CALCULATION .......................................................................................................................... 46
10. LIQUID VISCOSITY MEASUREMENT USING CAPILLARY TYPE VISCOMETER ..................................... 47
10.1. DESCRIPTION:....................................................................................................................... 47
10.2. Definitions............................................................................................................................ 47
10.3. Procedure: ........................................................................................................................... 47
10.4. Calculation and report: ......................................................................................................... 48
11. MUD WEIGHT, MARSH FUNNEL VISCOSITY AND pH ..................................................................... 51
11.1. MUD WEIGHT OR DENSITY TEST ........................................................................................... 51
11.2. Calibration ........................................................................................................................... 51
11.3. Test Procedure ..................................................................................................................... 51
11.4. MARSH FUNNEL VISCOSITY:.................................................................................................. 52
11.4.1. THEORY ................................................................................................................................ 52
11.4.2. Test Equipment .................................................................................................................... 52
11.4.3. Calibration ........................................................................................................................... 52
11.4.4. Test Procedure ..................................................................................................................... 52
11.5. HYDROGEN ION CONCENTRATION (pH) ................................................................................ 52
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 11.5.1. THEORY ................................................................................................................................ 52
11.5.2. METHODS OF MEASURING PH IN THE LABORATORY ............................................................. 53
11.5.3. LABORATORY EXPERIMENT .................................................................................................. 53
11.6. QUESTIONS .......................................................................................................................... 54
12. MUD RHEOLOGY TEST .................................................................................................................. 55
12.1. INTRODUCTION .................................................................................................................... 55
12.2. VISCOSITY............................................................................................................................. 55
12.2.1. Theory.................................................................................................................................. 55
12.2.2. Test Equipment .................................................................................................................... 55
12.2.3. Test Procedure ..................................................................................................................... 56
12.2.4. Rheological Calculations ....................................................................................................... 56
12.3. GEL STRENGTH: .................................................................................................................... 56
12.3.1. THEORY ................................................................................................................................ 56
12.3.2. Test Procedures ................................................................................................................... 56
12.4. YIELD POINT ......................................................................................................................... 57
12.4.1. THEORY ................................................................................................................................ 57
12.4.2. Calculation: .......................................................................................................................... 57
12.4.3. EXPERIMENT ........................................................................................................................ 57
12.5. QUESTIONS .......................................................................................................................... 57
13. FILTRATION, WALL BUILDING, AND RESISTIVITY ........................................................................... 58
13.1. FILTRATION THEORY ............................................................................................................. 58
13.2. Test Equipment .................................................................................................................... 58
13.3. Test Procedure for Filtration Rate At 100 Psi & Room Temperature ...................................... 59
13.4. WALL BUILD ......................................................................................................................... 59
13.4.1. MEASUREMENT PROCEDURE FOR MUD CAKE THICKNESS .................................................... 59
13.5. MUD RESISTIVITY ................................................................................................................. 59
13.5.1. THEORY ................................................................................................................................ 59
13.6. Measurement Procedure for Mud Cake Resistivity ............................................................... 60
13.7. Measurement Procedure For Mud Filtrate Resistivity ........................................................... 60
13.8. QUESTIONS .......................................................................................................................... 61
14. CONTROL OF MUD WEIGHT ......................................................................................................... 61
14.1. EFFECT OF ADDING WEIGHT MATERIAL (BARITE) .................................................................. 61
14.1.1. THEORY ................................................................................................................................ 61
14.1.2. Test Procedure ..................................................................................................................... 61
14.2. EFFECT OF ADDING BENTONITE ON MUD PROPERTIES FOR FRESH AND SALT WATER BASE
MUD: 62

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 14.2.1. Procedure ............................................................................................................................ 62
14.3. WATER-BACK (ADDING WATER TO A CHEMICALLY TREATED MUD)....................................... 62
14.4. QUESTIONS .......................................................................................................................... 62
15. SOLID & LIQUID CONTENT AND EMULSION CHARACTERISTICS OF DRILLING FLUID ....................... 63
15.1. SAND CONTENT DETERMINATION ........................................................................................ 63
15.1.1. Theory.................................................................................................................................. 63
15.1.2. Test Equipment: ................................................................................................................... 63
15.1.3. Test Procedure ..................................................................................................................... 63
15.2. EMULSION TEST ................................................................................................................... 64
15.2.1. THEORY ................................................................................................................................ 64
15.2.2. Test Procedure ..................................................................................................................... 64
15.3. OIL, WATER, SOLID & CLAY CONTENT DETERMINATION:....................................................... 64
15.3.1. THEORY ................................................................................................................................ 64
15.3.2. Test Equipment .................................................................................................................... 65
15.3.3. Test Procedure ..................................................................................................................... 65
15.4. THEORY AND CALCULATIONS OF SOLID CONTENT ................................................................ 66
15.5. QUESTIONS .......................................................................................................................... 67
16. OIL WELL CEMENTING EXPERIMENT............................................................................................. 68
16.1. WATER RATIOS FOR PORTLAND CEMENT SLURRY ................................................................. 68
16.1.1. Objective .............................................................................................................................. 68
16.1.2. Test Equipment .................................................................................................................... 68
16.2. FREE WATER SEPARATION TEST PROCEDURE ........................................................................ 68
16.3. NORMAL & MINIMUM WATER CONTENT OF CEMENT SLURRY: ............................................ 69
16.3.1. Test Procedure ..................................................................................................................... 69
17. THICKENING TIME TEST:............................................................................................................... 70
17.1. Definition ............................................................................................................................. 70
17.2. Test Procedure ..................................................................................................................... 70

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1. LABORATORY SAFETY
1.1. FIVE PRINCIPLES OF SAFETY
The Laboratory Safety Program incorporates the following principles:

1. Practice safety
2. Safety of others
3. Hazards associated with your particular experiment
4. What to do in an emergency
5. Report hazards or hazardous conditions

1.3.1 PRACTICE SAFETY

In order to have an effective safety program, some common basic rules must be established.
Some of the more basic safety practices that you are expected to follow are:

a) Wear appropriate eye protection whenever working with any potential eye hazards.
b) Use a hood for hazardous, volatile, and noxious chemicals.
c) Label an experiment to show its associated dangers and the persons to contact in case
of a danger.

1.3.2 SAFETY OF OTHERS

Your concern for safety must include the people around you. Your experiment must be safely
maintained so that everyone in the area is amply protected and warned of inherent dangers.
In addition, this principle of looking out for the other person should include the practice of
pointing out unsafe procedures to those people committing the unsafe act. Another aspect of
this second principle involves alerting those around you in case of an accident. It is your
responsibility to alert personnel in the immediate vicinity of a fire or an emergency!

1.3.3 HAZARDS ASSOCIATED WITH YOUR PARTICULAR EXPERIMENT

Prevention is the key to safety. Prior to any experiment, it is wise to consider the potential
hazards and safety precautions involved in the work. Hazards may include toxic substances,
electrical circuits, mechanical equipment and waste chemicals. Safety precautions include
correct materials handling and proper equipment operation.

1.3.4 WHAT TO DO IN AN EMERGENCY

You must be prepared to respond quickly and precisely to an emergency. You must familiarize
yourself with the laboratory you are working in, its exits, and its associated safety equipment:
eyewash stations, showers, sinks, fire extinguishers, and spill kits. Just a few moments spent
learning the locations and use of these pieces of equipment prior to an emergency could save
a life.

If the emergency is of an infiltrating nature, such as a fire, gas leak, or release of toxic fumes,
the following procedures should be followed:

• Alert personnel in the immediate vicinity

• Confine the fire or emergency, if possible
• Summon aid
• Evacuate the building
• Report pertinent information to responding emergency personnel.

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 1.3.5 REPORT HAZARDS OR HAZARDOUS CONDITIONS
You must report any incident to the Lab Technician without delay. The remainder of this
Safety Manual presents examples of hazards that you are likely to encounter in the laboratory
and what you should know about them to minimize their danger to you and to others.

1.2. FIRST AID

There are certain serious injuries in which time is so important that treatment must be started
immediately.

1.3.6 STOPPAGE OF BREATHING

For stoppage of breathing (e.g. from electrical shock or asphyxiation), the mouth-to-mouth
method of resuscitation is far superior to any other known. If victim is found unconscious on
the floor and not breathing, rescue breathing must be started at once, seconds count.

1.3.7 SEVERE BLEEDING

Severe bleeding can almost always be controlled by firm and direct pressure on the wound
with a pad or cloth. The cleaner the cloth, the more desirable it is; however, in an emergency,
use part of the clothing. In addition:

1. Wrap the injured to avoid shock and call immediately for medical attention.
2. Raise the bleeding part higher than the rest of the body and continue to apply
direct pressure.
3. Keep victim lying down.

1.3.8 THERMAL BURNS

1. If the burn is minor, apply ice or cold water.
2. In case of clothing fire:
a. The victim should drop to the floor and roll. A fire blanket, if nearby, should be
used to smother the flames.
b. After flames are extinguished, deluge the injured under a safety shower,
removing any clothing contaminated with chemicals.
c. Keep the water running on the burn for several minutes to remove heat and
wash area.
d. Place clean, soaking wet, ice-packed cloth on burned areas.
e. Never use a fire extinguisher on a person with burning clothing.

1.3.9 TRAUMATIC SHOCK

In cases of traumatic shock, or where the nature of the injury is not clear, keep the victim
warm, lying down and quiet. Wait until medical assistance arrives before moving the victim.
One should treat all injuries as potential shock situations, as they may turn into one. Some
common symptoms of shock are cold and clammy skin, paleness, and deliria.

1.3. SAFETY RULES

1.3.10 PERSONAL PRECAUTIONS
1. Avoid working alone in the laboratory: An individual is advised to work only under
supervision of the Technician.
2. Eye protection: In order to work safely, you must certainly protect your eyes. This
can be achieved by wearing safety glasses or mask.

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 3. Usage of mask: Suitable masks should be used in case of breathing in hazardous
materials.
4. Clothing: Wearing lab coats is necessary. Shorts and open-toed shoes are not
recommended when working in the lab. Never wear loose clothing in the lab.
5. Hand protection: For any laboratory procedure requiring the use of clothes, make
sure you are using gloves made of a material suitable for the operation.
6. Food and beverages: Consumption of food and beverages in the labs is not
permitted.
7. Personal hygiene: Wash hands and arms prior to leaving the laboratory.

1.3.11 LABORATORY PRACTICE

A. HAZARDOUS CHEMICALS
1. All containers must be labelled.
2. Do not use chemical from unlabelled containers.
3. Never taste or smell any chemical.
4. Clean spills immediately.
5. Avoid direct contact with any chemical. What might be considered safe today may
eventually be found to be harmful.
B. GLASSWARE
1. Never use cracked or chipped glassware.
2. Insert tubing properly into stoppers.
C. EQUIPMENT
2. Before using an instrument or machine, be sure you have been instructed and
authorized by the person responsible for the equipment.
3. Become familiar with potential hazards associated with the equipment, emergency
shut down procedures, as well as the operating procedures.
4. Check all electrical connections and check that all rotating parts are free to turn.
5. Laboratory equipment should not be placed in corridors.

Gas Cylinders
1. Do not use an open flame near gas cylinders.
2. Before using gas in an experiment, be sure there are no leaks in the system.
3. Learn directions for closing and opening valves.
4. Familiarize yourself with the toxic properties of each gas you work with.
D. TRANSPORTING CHEMICALS

Chemicals should not be carried in open containers in the lab.

1.4. CHEMICAL HAZARDS AND SAFETY PROCEDURES

1.5. UNATTENDED CHEMICAL REACTIONS
Take great care in setting up chemical reactions that are to be left unattended for any period
of time. Note that unattended operation should be avoided if at all possible. The possible
hazards that might arise from failure of a heating mantle, failure of a water cooling system,
and failure of an exhaust, are obvious points to check before leaving a reaction unattended.
The experimenter should also notify his/her advisor that the experiment will be running
overnight.

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 1.6. TOXIC HAZARDS
Researchers should be aware of the toxic hazards of the materials they are using, and those
being used by others their vicinity. Care should be taken to prevent toxic materials that may
enter the body through the skin, inhalation or ingestion.

1.7. ORGANIC SOLVENTS

Many organic solvents possess harmful vapours for human health. These organic solvents are
also volatile and the vapours are flammable. One should be aware of the hazards, and safety
precautions while using these solvents.

Acetone: Possesses toxic and flammable vapours. Use proper ventilation, safety glasses and
gloves

Methanol: Possesses harmful vapours that can cause dizziness, central nervous system
depression and shortness of breath. So it should be used in a ventilated hood and neoprene
gloves should be worn.

Benzene: Carcinogenic. Chronic poisoning can occur by inhalation of relatively small amounts
over a long time. It can also be absorbed through the skin. Vapours are flammable and it
should be stored carefully.

1.8. CHEMICAL WASTE DISPOSAL

Each individual has the responsibility for seeing that laboratory waste chemicals are safely
collected, identified, stored for disposal, and that anyone involved is fully advised of the need
for any special methods or facilities for proper disposal. Disposal of chemical waste down the
drain to the sanitary sewer systems is hazardous. Material flushed to the sewer can be
dangerous to maintenance personnel and the public. Chemical vapours and odours can
recirculate back into the buildings.

When collecting compatible solvents in the same container do not mix halogenated and
nonhalogenated solvents. The container must have all the ingredients and concentrations
listed on the outside.

1.9. ELECTRICAL HAZARDS AND SAFETY PROCEDURES

While electricity is in constant use by the researcher, both within and outside the laboratory,
significant physical harm or death may result from its misuse. With direct current, a man can
detect a “tingling” feeling at 1 mA and the median “let-go” threshold (the current at which he
cannot release the conductor) is 76 mA. For 60 Hertz alternating current, the values are 0.4
mA and 16 mA, respectively. Women are more sensitive to the effect of electrical current.
Higher currents produce respiratory inhibition, then ventricular fibrillation, and ultimately
cardiac arrest. If an electrical hazard is suspected, the device in question should be
disconnected immediately and the cause ascertained by a person competent in such matters.

1.10. PRECAUTIONS
Multi-strip outlets should not be used in place of permanently installed receptacles. If
additional outlets are required have them installed by an electrician.

1. Turn off the power to equipment before inspecting it. Turn off circuit breakers or
unplug the equipment.

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 2. Use only tools and equipment with non-conducting handles when working with
electrical devices.
3. When checking an operating circuit keep one hand either in a pocket or behind back
to get the extra style points from the Russian judge (to avoid making a closed circuit
through the body).
4. Never change wiring with circuit plugged into power source.
5. Avoid contacting circuits with wet hands.
6. Check circuits for proper grounding with respect to the power source.
7. Keep the use of extension cords to a minimum and cords as short as possible.
8. Do not use or store highly flammable solvents near electrical equipment.
9. Maintain a work space clear of extraneous material such as books, papers, and clothes.
10. Do not insert another fuse of larger capacity if an instrument keeps blowing fuses - this
is a symptom requiring expert repairs. If a fuse blows, find the cause of the problem
before putting in another one.

1.11. STATIC ELECTRICITY AND SPARK HAZARDS

Sparks may result in explosion in areas where flammable liquids are being used and therefore
proper grounding of equipment and containers is necessary.

Some common potential sources of spark are:

1. The making and breaking of an electrical circuit when the circuit is energized
2. Metal tanks and containers
3. Plastic lab aprons
4. Metal clamps, nipples, or wire used with non-conducting hoses
5. High pressure gas cylinders upon discharge

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2. INTRODUCTION
Knowledge of petrophysical and hydrodynamic properties of reservoir rocks are of
fundamental importance to the petroleum engineer. These data are obtained from two major
sources: core analysis and well logging. In this book we present some details about the
analysis of cores and review the nature and quality of the information that can be deduced
from cores.

Cores are obtained during the drilling of a well by replacing the drill bit with a diamond core
bit and a core barrel. The core barrel is basically a hollow pipe receiving the continuous rock
cylinder, and the rock is inside the core barrel when brought to surface. Continuous
mechanical coring is a costly procedure due to:

- The drill string must be pulled out of the hole to replace the normal bit by core bit and
core barrel.
- The coring operation itself is slow.
- The recovery of rocks drilled is not complete.
- A single core is usually not more than 9 m long, so extra trips out of hole are required.

Coring should therefore be a detailed programmed, especially in production wells. In an

exploration well the coring cannot always be accurately planned due to lack of knowledge
about the rock. Now and then there is a need for sample in an already drilled interval, and
then sidewall coring can be applied. In sidewall coring a wireline-conveyed core gun is used,
where a hollow cylindrical “bullet” is fired in to the wall of the hole. These plugs are small and
usually not very valuable for reservoir engineers.

During drilling, the core becomes contaminated with drilling mud filtrate and the reduction
of pressure and temperature while bringing the core to surface results in gas dissolution and
further expansion of fluids. The fluid content of the core observed on the surface cannot be
used as a quantitative measure of saturation of oil, gas and water in the reservoir. However,
if water based mud is used the presence of oil in the core indicates that the rock information
is oil bearing.

When the core arrives in the laboratory plugs are usually drilled 20-30 cm apart throughout
the reservoir interval. All these plugs are analysed with respect to porosity, permeability,
saturation and lithology. This analysis is usually called routine core analysis. The results from
routine core analysis are used in interpretation and evaluation of the reservoir. Examples are
prediction of gas, oil and water production, definition of fluid contacts and volume in place,
definition of completion intervals etc. Data from routine core analysis and from
supplementary tests and the application of these data area summarized in Table 1.1.

13
Table 2-1:Routine core analysis and supplementary measurements.

Data Application
Routine core analysis
Porosity Storage capacity
Permeability Flow capacity
Saturations Define the mobile hydrocarbons (productive zones and
contacts), type of hydrocarbons
Lithology Rock type and characteristics (fractures, layering etc.)
Supplementary measurement
Vertical permeability Effect of coning, gravity drainage etc.
Core-gamma surface log Identify lost core sections, correlate cores and logs
Matrix density Calibrate the density log
Oil and water analysis Densities, viscosities, interfacial tension, composition
etc.

Special core analysis includes several measurements with the objective of obtaining detailed
information about multiphase flow behaviour. Special core analysis gives information about
the distribution of oil, gas, and water in the reservoir (capillary pressure data), residual oil
saturation and multiphase flow characteristics (relative permeabilities). Measurements of
electrical and acoustic properties are occasionally included in special core analysis. This
information is mainly used in the interpretation of well logs.

The effect of pressure and temperature on rock and fluid properties is in some reservoir
formations significant, and laboratory measurements should therefore be made at, or
corrected to, reservoir conditions wherever possible. Included in special core analysis is in
some cases detailed petrographical analysis of rocks (grain size distribution, clay
identification, diagenesis etc.). Wettability analysis and special tests for enhanced oil recovery
(EOR) are also often part of special core analysis. Table 1.2 is a list of the various special core
analysis tests.
Table 2-2: Special core analysis

Tests/Studies Data/Properties
Static tests
Compressibility studies Permeability and porosity vs. pressure
Petrographical studies Mineral identification, diagenesis, clay identification,
grain size distribution, pore geometry etc.
Wettability Contact angle and wettability index
Capillarity Capillary pressure vs. saturation
Acoustic tests
Electric tests
Dynamic tests
Flow studies Relative permeability and end point saturations
EOR-Flow tests Injectivity and residual saturation
14
 CORE
AND
ROCK
PROPERTIES
LAB

15
3. ROCK SAMPLE PREPARATION

3.1. CLEANING AND SATURATION DETERMINATION

3.2. OBJECTIVES
Cleaning, drying and saturation determination of the core samples

3.3. INTRODUCTION AND THEORY

Before measuring porosity and permeability, the core samples must be cleaned of residual
fluids and thoroughly dried. The cleaning process may also be apaert of fluid saturation
determination.

3.4. LABORATORY METHODS

3.5. DIRECT INJECTION OF SOLVENT
The solvent is injected into the sample in a continuous process. The sample is held in a
rubber sleeve thus forcing the flow to be uniaxial.

CENTRIFUGE FLUSHING
A centrifuge which has been fitted with a special head sprays warm solvent onto the sample.
The centrifugal force then moves the solvent through the sample. The used solvent can be
collected and recycled.

GAS DRIVEN SOLVENT EXTRACTION

The sample is placed in a pressurized atmosphere of solvent containing dissolved gas. The
solvent fills the pores of sample. When the pressure is decreased, the gas comes out of
solution, expands, and drives fluids out of the rock pore space. This process can be repeated
as many times as necessary.

SOXHLET EXTRACTION
A Soxhlet extraction apparatus is the most common method for cleaning sample, and is
routinely used by most laboratories. As shown in Figure 2.1a, toluene is brought to a slow boil
in a Pyrex flask; its vapours move upwards and the core becomes engulfed in the toluene
vapors (at approximately 110°C). Eventual water within the core sample in the thimble will
be vaporized. The toluene and water vapours enter the inner chamber of the condenser, the
cold water circulating about the inner chamber condenses both vapours to immiscible liquids.
Recondensed toluene together with liquid water falls from the base of the condenser onto the
core sample in the thimble; the toluene soaks the core sample and dissolves any oil with which
it come into contact. When the liquid level within the Soxhlet tube reaches the top of the
siphon tube arrangement, the liquids within the Soxhlet tube are automatically emptied by a
siphon effect and flow into the boiling flask. The toluene is then ready to start another cycle.

A complete extraction may take several days to several weeks in the case of low API gravity
crude or presence of heavy residual hydrocarbon deposit within the core. Low permeability
rock may also require a long extraction time.

DEAN-STARK DISTILLATION-EXTRACTION
The Dean-Stark distillation provides a direct determination of water content. The oil and
water area extracted by dripping a solvent, usually toluene or a mixture of acetone and
16
chloroform, over the plug samples. In this method, the water and solvent are vaporized,
recondensed in a cooled tube in the top of the apparatus and the water is collected in a
calibrated chamber (Figure 2.1b). The solvent overflows and drips back over the samples. The
oil removed from the samples remains in solution in the solvent. Oil content is calculated by
the difference between the weight of water recovered and the total weight loss after
extraction and drying.

Fig. 3.1: Schematic diagram of Soxhlet (a) and Dean- Stark (b) apparatus.

VACUUM DISTILLATION
The oil and water content of cores may be determined by this method. As shown in Figure 3.2,
a sample is placed within a leakproof vacuum system and heated to a maximum temperature
of 230°C. Liquids within the sample are vaporized and passed through a condensing column
that is cooled by liquid nitrogen.

Fig. 3.2: Vacuum distillation Apparatus.

17
 3.6. SUMMARY
The direct-injection method is effective, but slow. The method of flushing by using centrifuge
is limited to plug-sized samples. The samples also must have sufficient mechanical strength
to withstand the stress imposed by centrifuging. However, the procedure is fast. The gas
driven-extraction method is slow. The disadvantage here is that it is not suitable for poorly
consolidated samples or chalky limestones. The distillation in a Soxhlet apparatus is slow, but
is gentle on the samples. The procedure is simple and very accurate water content
determination can be made. Vacuum distillation is often used for full diameter cores because
the process is relatively rapid. Vacuum distillation is also frequently used for poorly
consolidated cores since the process does not damage the sample. The oil and water values
are measured directly and dependently of each other.

In each of these methods, the number of cycles or amount of solvent which must be used
depends on the nature of the hydrocarbons being removed and the solvent used. Often, more
than one solvent must be used to clean a sample. The solvents selected must not react with
the minerals in the core. The commonly used solvents are:

- Acetone
- Benzene
- Benzen-methol Alcohol
- Carbon-tetrachloride
- Chloroform
- Methylene Dichloride
- Mexane
- Naphtha
- Tetra Chloroethylene
- Toluene
- Trichloro Ethylene
- Xylene

Toluene and benzene are most frequently used to remove oil and methanol and water is used
to remove salt from interstitial or filtrate water. The cleaning procedures used are specifically
important in special core analysis tests, as the cleaning itself may change wettabilities.

The core sample is dried for the purpose of removing connate water from the pores, or to
remove solvents used in cleaning the cores. When hydratable minerals are present, the drying
procedure is critical since interstitial water must be removed without mineral alteration.
Drying is commonly performed in a regular oven or a vacuum oven at temperatures between
50°C to 105°C. If problems with clay are expected, drying the samples at 600C and 40 %
relative humidity will not damage the samples.

3.7. SATURATION DETERMINATION

DEFINITIONS
Fluid saturation is defined as the ratio of the volume of fluid in a given core sample to the pore
volume of the sample

18
 𝑉𝑤 𝑉𝑜 𝑉𝑔
𝑆𝑤 = 𝑆𝑜 = 𝑆𝑔 = (3.1)
𝑉𝑝 𝑉𝑝 𝑉𝑝

𝑆𝑤 + 𝑆𝑜 + 𝑆𝑔 = 1 (3.2)

where Vw, Vo, Vg and Vp are water, oil, gas and pore volumes respectively and S w, So and Sg are
water, oil and gas saturations. Note that fluid saturation may be reported either as a fraction
of total porosity or as a fraction of effective porosity. Since fluid in pore spaces that are not
interconnected cannot be produced from a well, the saturations are more meaningful if
expressed on the basis of effective porosity. The weight of water collected from the sample is
calculated from the volume of water by the relationship

𝑊𝑤 = 𝜌𝑤 𝑉𝑤 (3.3)

where ρw is water density in g/cm3. The weight of oil removed from the core may be computed
as the weight of liquid less weight of water

𝑊𝑜 = 𝑊𝐿 − 𝑊𝑤 (4.4)

where WL is the weight of liquids removed from the core sample in gram. Oil volume may then
be calculated as Wo/ρo. Pore volume Vp is determined by a porosity measurement, and oil and
water saturation may be calculated by Eq. (3.1). Gas saturation can be determined using Eq.
(3.2)

3.8. SATURATION DETERMINATION, DEAN-STARK DISTILLATION METHOD

(EXPERIMENT 1)
DESCRIPTION
The objective of the experiment is to determine the oil, water and gas saturation of a core
sample.

PROCEDURE
1. Weigh a clean, dry thimble. Use tongs to handle the thimble.
2. Place the cylindrical core plug inside the thimble, then quickly weigh the thimble and
sample.
3. Fill the extraction flask two-thirds full with toluene. Place the thimble with sample into
the long neck flask.
4. Tighten the ground joint fittings, but do not apply any lubricant for creating tighter
joints. Start circulating cold water in the condenser.
5. Turn on the heating jacket or plate and adjust the rate of boiling so that the reflux from
the condenser is a few drops of solvent per second. The water circulation rate should
be adjusted so that excessive cooling does not prevent the condenser solvent from
reaching the core sample.
6. Continue the extraction until the solvent is clear. Change solvent if necessary.
7. Read the volume of collected water in the graduated tube. Turn off the heater and
cooling water and place the sample into the oven (from 105°C to 120°C), until the
sample weight does not change. The dried sample should be stored in a desiccator.
8. Obtain the weight of the thimble and the dry core.
9. Calculate the loss in weight WL, of the core sample due to the removal of oil and water.
19
 10. Measure the density of a separate sample of the oil.
11. Calculate the oil, water and gas saturations after the pore volume V p of the sample is
determined.

DATA AND CALCULATIONS:

Sample No: Porosity, φ:

Worg Wdry ρw ρo Vw Wo Vo Vp So Sw Sg
g g g/cm g/cm cm3
3 3 g cm3 cm3

Where

Worg: Weight of original saturated sample

Wdry: Weight of desaturated and dry sample

Equations:

𝑊𝐿 = 𝑊𝑜𝑟𝑔 − 𝑊𝑑𝑟𝑦

𝑊𝑜 = 𝑊𝐿 − 𝑊𝑤

𝑉𝑏 = 𝜋(𝐷/2)2 𝐿

𝑉𝑝 = 𝜑𝑉𝑏

where D and L are diameter and length of the core sample, respectively.

20
4. POROSITY

4.1. DEFINITIONS
From the viewpoint of petroleum engineers, the two most important properties of a reservoir
rock are porosity and permeability. Porosity is a measure of storage capacity of a reservoir. It
is defined as the ratio of the pore volume to bulk volume, and is may be expressed as either a
percent or a fraction. In equation form
𝑝𝑜𝑟𝑒 𝑣𝑜𝑙𝑢𝑚𝑒 𝑏𝑢𝑙𝑘 𝑣𝑜𝑙𝑢𝑚𝑒 − 𝑔𝑟𝑎𝑖𝑛 𝑣𝑜𝑙𝑢𝑚𝑒
𝜑= = (4.1)
𝑏𝑢𝑙𝑘 𝑣𝑜𝑙𝑢𝑚𝑒 𝑏𝑢𝑙𝑘 𝑣𝑜𝑙𝑢𝑚𝑒
Two types of porosity may be measured: total or absolute porosity and effective porosity.
Total porosity is the ratio of all the pore spaces in a rock to the bulk volume of the rock.
Effective porosity φe is the ratio of interconnected void spaces to the bulk volume. Thus, only
the effective porosity contains fluids that can be5 produced from wells. For granular materials
such as sandstone, the effective porosity may approach the total porosity, however, for shales
and for highly cemented or vugular rocks such as some limestones, large variations may exist
between effective and total porosity.

Porosity may be classified according to its origin as either primary or secondary. Primary or
original porosity is developed during deposition of the sediment. Secondary porosity is
caused by some geologic process subsequent to formation of the deposit. These changes in
the original pore spaces may be created by ground stresses, water movement, or various types
of geological activities after the original sediments were deposited. Fracturing or formation
of solution cavities often will increase the original porosity of the rock.

Figure 4.1-1: Cubic packing (a), rhombohedral (b), cubic packing with two grain sizes (c), and typical
sand with irregular grain shape (d).

For a uniform rock grain size, porosity is independent of the size of the grains. A maximum
theoretical porosity of 48% is achieved with cubic packing of spherical grains, as shown in
Fig. 4.1a. Rhombohedral packing, which is more representative of reservoir conditions, is
shown in Fig. 4.1b; the porosity for this packing is 26%. If a second, -smaller size of spherical
grains is introduced into cubic packing (Fig. 4.1c), the porosity decreases from 48% to 14%.
Thus, porosity is dependent on the grain size distribution and the arrangement of the grains,

21
as well as the amount of cementing materials. Not all grains are spherical, and grain shape
also influences porosity. A typical reservoir sand is illustrated in Fig. 4.1d.

4.2. EFFECT OF COMPACTION ON POROSITY

Compaction is the process of volume reduction due to an externally applied pressure. For
extreme compaction pressures, all materials show some irreversible change in porosity. This
is due to distortion and crushing of the grain or matrix elements of the materials, and in some
cases, recrystallization. The variation of porosity with change in pressure can be represented
by

𝜑2 = 𝜑2 𝑒 𝐶𝑓 (𝑃2 −𝑃1) (4.2)

where φ2 and φ1 are porosities at pressure P2 and P1 respectively, and Cf is formation

compressibility. Formation compressibility is defined as summation of both grain and pore
compressibility. For most petroleum reservoirs, grain compressibility is considered to be
negligible. Formation compressibility can be expressed as
1 𝑑𝑉
𝐶𝑓 = (4.3)
𝑉 𝑑𝑃
where dP is change in reservoir pressure. For porous rocks, the compressibility depends
explicitly on porosity

4.3. POROSITY MEASUREMENTS ON CORE PLUGS

From the definition of porosity, it is evident that the porosity of a sample of porous material
can be determined by measuring any two of the three quantities: Bulk volume, pore volume
or grain volume. The porosity of reservoir rock may be determined by

- Core analysis
- Well logging technique
- Well testing

The question of which source of porosity data is most reliable cannot be answered without
reference to a specific interpretation problem. These techniques can all give correct porosity
values under favourable conditions. The core analysis porosity determination has the
advantage that no assumption need to be made as to mineral composition, borehole effects,
etc. However, since the volume of the core is less than the rock volume which is investigated
by a logging device, porosity values derived from logs are frequently more accurate in
heterogeneous reservoirs.

In the following sections we will discuss how to estimate pore-, grain-, and bulk-volumes
from core plugs.

4.4. BULK VOLUME MEASUREMENT

Although the bulk volume may be computed from measurements of the dimensions of a
uniformly shaped sample, the usual procedure utilises the observation of the volume of fluid
displaced by the sample. The fluid displaced by a sample can be observed either
volumetrically or gravimetrically. In either procedure it is necessary to prevent the fluid
penetration into the pore space of the rock. This can be accomplished (1) by coating the
22
sample with paraffin or a similar substance, (2) by saturating the core with the fluid into
which it is to be immersed, or (3) by using mercury.

Gravimetric determinations of bulk volume can be accomplished by observing the loss in

weight of the sample when immersed in a fluid or by change in weight of a pycnometer with
and without the core sample.

4.5. PORE VOLUME MEASUREMENT

All the methods measuring pore volume yield effective porosity. The methods are based on
either the extraction of a fluid from the rock or the introduction of a fluid into the pore spaces
of the rock.

One of the most used methods is the helium technique, which employs Boyle’s law. The
helium gas in the reference cell isothermally expands into a sample cell. After expansion, the
resultant equilibrium pressure is measured. The Helium porosimeter apparatus is shown
schematically in Fig. 4.2.

Figure 4.3-1: Schematic diagram of helium porosimeter apparatus.

Helium has advantages over other gases because: (1) its small molecules rapidly penetrate
small pores, (2) it is inert and does not adsorb on rock surfaces as air may do, (3) helium can
be considered as an ideal gas (i.e., z = 1.0) for pressures and temperatures usually employed
in the test, and (4) helium has a high diffusivity and therefore affords a useful means for
determining porosity of low permeability rocks.

The schematic diagram of the helium porosimeter shown in Fig. 5.2 has a reference volume
V1, at pressure p1, and a matrix cup with unknown volume V2, and initial pressure p2. The
reference cell and the matrix cup are connected by tubing; the system can be brought to
equilibrium when the core holder valve is opened, allowing determination of the unknown
volume V2 by measuring the resultant equilibrium pressure p. (Pressure p1 and p2 are
controlled by the operator; usually p1 = 100 and p2 = 0 psig). When the core holder valve is
opened, the volume of the system will be the equilibrium volume V, which is the sum of the
volumes V1 and V2. Boyle’s law is applicable if the expansion takes place isothermally. Thus
the pressure-volume products are equal before and after opening the core holder valve:

𝑝1 𝑉1 + 𝑝2 𝑉2 = 𝑝(𝑉1 + 𝑉2 ) (4.4)
23
Solving the equation for the unknown volume, V2:
(𝑝 − 𝑝1 )𝑉1
𝑉2 = (4.5)
𝑝2 − 𝑝

Since all pressures in equation (5.4) must be absolute and it is customary to set p1 = 100 psig
and p2 = 0 psig, Eq. (5.4) may be simplified as follows:
𝑉1 (100 − 𝑝)
𝑉2 = (4.6)
𝑝

where V2 in cm3 is the unknown volume in the matrix cup, and V1 in cm3 is the known volume
of the reference cell. p in psig is pressure read directly from the gauge.

Small volume changes occur in the system, including the changes in tubing and fittings caused
by pressure changes during equalization. A correction factor, G, may be introduced to correct
for the composite system expansion. The correction factor G is determined for porosimeters
before they leave the manufacturer, and this correction is built into the gauge calibration in
such a way that it is possible to read the volumes directly from the gauge.

Another method of pore volume determination is to saturate the sample with a liquid of
known density, and noting the weight increase (gravimetric method).

When a rock has a small fraction of void space, it is difficult to measure porosity by the
mentioned methods. At this case, mercury injection is used. The principle consists of forcing
mercury under relatively high pressure in the rock pores. A pressure gauge is attached to the
cylinder for reading pressure under which measuring fluid is forced into the pores. Fig. 5.3b
shows a typical curve from the mercury injection method. The volume of mercury entering
the core sample is obtained from the device with accuracy up to 0.01 cm 3.

Figure 4.3-2: Mercury injection pump (a) and porosity through mercury injection (b).

24
 4.6. GRAIN VOLUME MEASUREMENT
The grain volume of pore samples is sometimes calculated from sample weight and
knowledge of average density. Formations of varying lithology and, hence, grain density limit
applicability of this method. Boyle’s law is often employed with helium as the gas to determine
grain volume. The technique is fairly rapid, and is valid on clean and dry sample.

The measurement of the grain volume of a core sample may also be based on the loss in weight
of a saturated sample plunged in a liquid.

Grain volume may be measured by crushing a dry and clean core sample. The volume of
crushed sample is then determined by (either pycnometer or) immersing in a suitable liquid.

4.7. EFFECTIVE POROSITY DETERMINATION BY HELIUM POROSIMETER

METHOD (EXPERIMENT 2)
DESCRIPTIONS
The helium porosimeter uses the principle of gas expansion, as described by Boyle’s law. A
known volume (reference cell volume) of helium gas, at a predetermined pressure, is
isothermally expanded into a sample chamber. After expansion, the resultant equilibrium
pressure is measured. This pressure depends on the volume of the sample chamber minus the
rock grain volume, and then the porosity can be calculated.

PROCEDURE
1. Measure the diameter and length of the core using calliper.
2. Give the porosimeter a helium supply, 10 bar.
3. Determine the volume of the matrix cup with core, V2:
3.1 Put the cleaned, dried core inside the matrix cup, and mount the cup in the cup
holder.
3.2 Open “source” and then “supply”.
3.3 Regulate the needle at 100.
3.4 Close “source” and then “supply”.
3.5 Open “core holder”.
3.6 Take the reading on TOP SCALE, V2 = cm3.
4. Determine the volume of the matrix cup without core, V1:
4.1 Take out the core from the matrix cup, and mount the cup in the cup holder.
4.2 Open “source” and then “supply”.
4.3 Open “cell 1”.
4.4 Regulate the needle at 100.
4.5 Close “source and then “supply”.
4.6 Open core “holder”.

Take the reading on MIDDLE SCALE, V1 = cm3.

CALCULATIONS AND REPORT

1. Calculate and fill the data form.

Core No.: D: cm, L: cm.

V2 (cm3) Vg (cm3) Vb (cm3)

25
 V1 (cm3) V2 (cm3) Vg (cm3) Vb (cm3) φe

where

V1 = the volume of the matrix cup without core, cm3.

V2 = the volume of the matrix cup with core, cm3.

Vg = V1-V2, the volume of grain and non-connected pores, cm3.

Vb = the bulk volume of core, cm3.

φe = (Vb - Vg)/ Vb effective (interconnected) porosity of the core, fraction.

4.8. POROSITY DETERMINATION BY LIQUID SATURATING METHOD

(EXPERIMENT 3)
DESCRIPTION
The determination of the effective liquid porosity of a porous plug is the initial part of the
measurement of capillary pressure using porous plate method in core laboratories. Before
the capillary pressure is determined the volume of the saturating liquid (brine or oil) in the
core must be known. Thus, the effective liquid porosity of the core can be calculated in the
beginning of capillary pressure measurement.

PROCEDURE
1. Weigh dry Berea plug Wdry, measure its diameter D, and length L, with calliper (1 core
for each group).
2. Put the cores in the beaker inside a vacuum container, run vacuum pump about 1 hour.
3. Saturate the cores with 36 g/l NaCl brine, ρbrine = 1.02g/cm3.

Weigh the saturated cores, Wsat.

CALCULATIONS AND REPORT:

1. Calculate the saturated brine weight, Wbrine = Wsat - Wdry.
2. Calculate the pore volume (saturated brine volume), Vp = Wsat / ρbrine.
3. Calculate effective porosity, φe = Vp / Vb.

Core No.: D: cm, L: cm.

Wdry (g) Wsat (g) Wbrine (g) Vp (cm3) φe

26
5. PERMEABILITY
5.1. DEFINITION
Permeability is a property of the porous medium and it is a measure of capacity of the medium
to transmit fluids. Permeability is a tensor that in general is a function of pressure. Usually,
the pressure dependence is neglected in reservoir calculations, but the variation with position
can be pronounced. Very often the permeability varies by several magnitudes, and such
heterogeneity will of course influence any oil recovery.

5.2. DARCY’S LAW

Darcy (1856) performed a series of experiments on the relationship effecting the downward
flow of water through sands. The generalised equation called Darcy’s law may be written in
the form

𝑘̿
𝑢̅ = − (∇𝑃 + 𝜌𝑔̅ ) (5.1)
𝜇

where 𝑢̅ is superficial velocity, 𝑘̿ is permeability tensor, µ is fluid viscosity, ∇P is pressure

gradient, ρ is fluid density and 𝑔̅ is gravitational vector. Writing flow velocity ν as the ratio of
volumetric rate to cross-sectional area perpendicular to flow q/A in distance L, Darcy’s law
can be expressed
𝑞 𝑘 ∆𝑃
=𝑣= (5.2)
𝐴 𝜇 𝐿

The dimensions of permeability can be established by substituting the units of the other in
the equation. The unit darcy results from the choice of cgs system units

𝑞[𝑐𝑚3 ⁄𝑠] 𝜇 [𝑐𝑝]𝐿[𝑐𝑚]

𝑑𝑎𝑟𝑐𝑦[𝐷] = (5.3)
∆[atm]A[𝑐𝑚2 ]

The permeability in SI system has dimension of m2.

5.3. KLINKENBERG EFFECT

Klinkenberg has reported variations in permeability determined by using gases as the flowing
fluid compared to those obtained when using non-reactive liquids. These variations were
considered to be due to slippage, a phenomenon well known with respect to gas flow in
capillary tubes. The phenomenon of gas slippage occurs when the diameter of the capillary
openings approach the mean free path of the gas. The mean free path of a gas is a function of
molecular size and the kinetic energy of the gas. Therefore, permeability of gas depends on
factors which influence the mean free path, such as temperature, pressure and the molecular
size of the gas.

Fig. 5.1 is a plot of the permeability of a porous medium as determined at various mean
pressures using three different gases. Note that for each gas a straight line is obtained for the
observed permeability as a function of the reciprocal of the mean pressure of the test. All the
lines when extrapolated to infinite mean pressure (1/Pm = 0) intercept the permeability axis
at a common point. This point is designated kL, or the equivalent liquid permeability.

27
Figure 5-1: Variation in gas permeability with mean pressure and type of gas.

Klinkenberg has related apparent permeability ka measured for gas for an average pressure
Pm to the true permeability kL by
𝑏
𝑘𝑎 = 𝑘𝐿 (1 + ) (5.4)
𝑃𝑚

where b is constant depending upon the average free movement λ of the molecule at Pm
4𝐶′𝜆𝑃𝑚
𝑏= (5.5)
𝑟
where r is channel radius and C’ ≈ 1.

5.4. IDEAL GAS FLOW

Darcy’s equation defining permeability is linked to laminar flow in porous media. This laminar
flow is not always achieved especially in gas flows. Let us suppose that there is a metal tube
filled with sand (Fig. 10.2). Upstream and downstream pressure P1 and P2 are constants.

Figure 5-2: Linear flow of an ideal gas in sand-filled tube.

The mass flow 𝑚̇ is the same in all slices and each slice is related to the volume flow rate Q by

𝑚̇ = 𝑄. 𝜌 (5.6)
28
where 𝜌 is gas density in the slice when pressure is 𝑃. Using Boyle’s law, relationship 𝜌 = 𝑏𝑃
can be applied where b is a constant. And then
1
𝑄= 𝑚̇ (5.7)
𝑏𝑃
By substituting 𝑄 in Darcy’s equation, a differential relation between 𝑃 and distance 𝑥 may be
obtained
𝜇 𝑚̇
𝑏𝑃𝑑𝑃 = 𝑑𝑥 (5.8)
𝐴𝑘
After integration for distance L
𝑏 2 𝜇 𝑚̇
(𝑃1 − 𝑃12 ) = 𝐿 (5.9)
2 𝐴𝑘
and taking into account that m = QbP , we get

𝐴𝑘 (𝑃12 − 𝑃12 )
𝑄𝑎𝑡𝑚 = (5.10)
𝜇𝐿 2𝑃𝑎𝑡𝑚

The gas flow is measured at atmospheric conditions, thus Patm = 1 atm.

5.5. HIGH VELOCITY FLOW

For high flow rates, Darcy’s law is not valid. The range of flow rate which laminar flow exists
is dependent on the Reynolds number which is a dimensionless quantity. The Reynolds
number for porous media is defined as
𝑑𝑣𝜌
𝑅𝑒∗ = (5.11)
𝜇

where ν is average velocity (q/A), ρ is fluid density, µ is fluid viscosity and d is the average
sand grain diameter. For example, in sand, transition from laminar to turbulent flow occurs
in the range of Reynolds number from 1 to 10.

Many models were suggested to replace or modify Darcy’s law for high-velocity flow. The
most accepted model for non-Darcy flow was proposed by Forchheimer in 1901

− 𝛻𝑃 = 𝑎𝜈 + 𝑏𝜈 2 (5.12)

where a and b are constants and ν = q/A. Later work resulted in an equation in terms of fluid
and rock properties
𝜇
− 𝛻𝑃 = 𝜈 + 𝛽𝜌𝜈 2 (5.13)
𝑘
where β is high velocity coefficient and µ, ρ are viscosity and density of the gas respectively.
The high velocity coefficient is a property of the formation rock that accounts for the deviation
from Darcy’s law which is more pronounced in gas flow than in oil flow. Many correlations for
β exist in the literature. Usually, β is taken as a property of the reservoir rock which may be
estimate from

29
 𝑐𝑜𝑛𝑠𝑡.
𝛽= (5.14)
𝑘𝛼
where α is constant which can be determined experimentally from a known permeable
formation.

5.6. MEASUREMENT OF PERMEABILITY

Permeability is measured by passing a fluid of known viscosity through a core sample of
measured dimensions and then measuring flow rate and pressure drop. Various techniques
are used for permeability measurements of cores, depending on sample dimensions and
shape, degree of consolidation, type of fluid used, ranges of confining and fluid pressure
applied, and range of permeability of the core. Two types of instruments are usually used in
the laboratory:

(a) Variable head permeameter, IFP type.

(b) Constant head permeameter, Core Laboratories type.

Permeability tests are performed on samples which have been cleaned and dried and a gas
(usually air) is used for flowing fluid in the test. This is because:
1. steady state is obtained rapidly,
2. dry air will not alter the minerals in the rock, and
3. 100% fluid saturation is easily obtained.

Measured values using constant head equipment range from a low of 0.1 mD to 20 D. Data
accuracy declines at high and low permeability values and is within ± 0.5% of true value
otherwise.

CONSTANT HEAD PERMEAMETER

This equipment is designed for plug or whole core permeability measurements. This
experiment may be used for single or multiphase, compressible fluid or liquid measurements
and can also be used under reservoir pressure and temperature.

Fig 5.3 shows a diagram of a constant head permeameter. Air is usually used as gas flow.
Upstream and downstream pressures are measured by manometers on both sides of the core
and air flow is measured by means of a calibrated outlet. Air permeability can then be
calculated using Eq. (5.10).

Hassler core holder may be used with this instrument. The Hassler system is an improvement
of the rubber plug system whose tightness is limited at certain pressures. The core is placed
in a flexible rubber tube (Fig. 5.4). The Hassler cell has these advantages:

- Excellent tightness.
- Can be used for samples of different sizes.
- Much higher pressure or ∆P can be used.
- Can be used for measuring relative permeability.

Darcy’s equation may be used for determining permeability of liquids. The volumetric flow
rate q is constant for liquids, because the density does not change during flow through the
core.
30
Figure 5-3: Schematic diagram of permeameter.

Figure 5-4: Hassler type core holder.

5.7. MEASUREMENT OF AIR PERMEABILITY (EXPERIMENT 4)

DESCRIPTION
The constant head permeameter with the Hassler cell is used to measure the air permeability.

PROCEDURE
The measured air permeability is influenced by the mean pressure Pm of the core. The mean
pressure is regulated by the upstream and downstream values on the sides of Hassler cell.
The rate is measured at atmospheric conditions with a mass flow meter in percent of
maximum rate which is 200 l/hour. Air viscosity as a function of temperature is shown in Fig.
5.5.

Four measurements of air permeability will be taken at different pressures. It is important to

keep the ∆P constant, because the air flow at the core sample must be laminar. It is best to
have relative little pressure difference, ∆P. To avoid turbulent flow, use a maximal ∆P = 0.2
bar.

31
 RESULTS AND CALCULATION:
1. Calculate air permeability from Eq. (10.16).
2. Plot k versus 1/Pm and calculate kL.
3. Calculate Klinkenberg constant b.

Inlet pressure Outlet pressure

1/Pm Rate in % Q1atm
P1 P2

Figure 5-5: Gas viscosity as a function of temperature.

5.8. ABSOLUTE PERMEABILITY MEASUREMENT OF WATER (EXPERIMENT 5)

DESCRIPTION
The objective of this experiment is to measure the absolute permeability of water using a
method based on the Darcy theory.

PROCEDURE
1. Weight a dry Berea plug Wdry, measure its diameter D and length L, with caliper.
Saturate the core with 36 g/l NaCl brine and weigh the plug, Wsat.
2. Mount the core in core holder.
3. Measure three flow rates under three driving pressures: 0.6, 0.8, 1.0, or 1.2 bar. Each
measurement collects water production Vw, in ∆T = 60 seconds.
4. Plot a line through the three ∆P-Vw data in a grid paper. Calculate the absolute
permeability kabs and absolute injectivity Iabs.

CALCULATIONS AND REPORT

Core No.: D: cm, L: cm, Wdry: g, Wsat: g.

Δ𝑇(𝑖) Δ𝑃(1) Δ𝑃(1) Δ𝑃(3) 𝑘𝑜𝑏𝑠 𝐼𝑜𝑏𝑠

32
 = 60" bar bar bar darcy cm/s.bar

Vw

Liquid data:

ρw = 1.020 g/cm3, µw = 1.04 cp

Iabs = Absolute (water) injectivity = Vw/(∆T. A. ∆P)

where Vw is volume of water produced in time ∆T.

CALCULATION OF KABS
kabs = (µwLVw )/(A∆T∆P)

(µ.L)/(k.A.∆T) = slope of the ∆P-Vw plot

A = Section area of the core, cm2

33
 FLUID
PROPERTIES
LAB

34
6. DETERMINING DENSITY USING THE PYCNOMETER
6.1. DENSITY
The density, r, is elementary physical property of matter. For a homogeneous object it is
defined as the ratio of its mass m to its volume V
𝑚
𝜌= (6.1)
𝑉
Numerically it represents the mass per unit volume of matter. As it follows from equation
[1], the SI unit of density is kg/m3. However, g/cm3 is another unit commonly used in a
laboratory. Its conversion is
𝑔 𝐾𝑔
3
= 1000 3 (6.2)
𝑐𝑚 𝑚
The volume of an object increases with increasing temperature, because of the matter’s
volumetric thermal expansion. Therefore, according to equation (6.1), the density of an
object depends on its temperature, higher temperature results in lower density.
Exception is water in temperature range 0-4 °C, for which the density increases with
increasing temperature. The density of a gas further depends on the pressure as well.
Nevertheless, this effect is negligible in a case of liquid and/or solid matter.
There are several experimental methods used for density determination of liquids.
We will learn how to use pycnometer in this assignment.

Density determination by pycnometer is a very precise method. It uses a working liquid

with well-known density, such as water. We will use distilled water, for which
temperature dependent values of density 𝜌H2O are shown in Table 1. The pycnometer
(Fig. 1) is a glass flask with a close-fitting ground glass stopper with a capillary hole
through it. This fine hole releases a spare liquid after closing a top-filled pycnometer and
allows for obtaining a given volume of measured and/or working liquid with a high
accuracy.
First we fill pycnometer with distilled water. According to equation (6.1), the volume of
water that is filling the pycnometer and the stopper is
𝑚𝐻2 𝑂
𝑉= (6.3)
𝜌𝐻2 𝑂
Where mH2O is experimentally determined weight of water (empty pycnometer weight
subtracted).
We repeat the procedure for the liquid with unknown density rL and determine its weight
mL (measured weight minus weight of empty pycnometer). Volume V obtained in this
measurement is the same as the volume of water determined from equation [3]. It follows
alternated equation.
𝑚𝐿
𝑉= (6.4)
𝜌𝐿
Combining equations (6.3) and (6.4)
𝑚𝐻2 𝑂 𝑚𝐿
= (6.5)
𝜌𝐻2 𝑂 𝜌𝐿
yields a relation that provides the density of measured liquid
𝑚𝐿
𝜌𝐿 .𝜌
𝑚𝐻2 𝑂 𝐻2 𝑂

35
Figure 6-1: The pycnometer

6.2. PRECAUTIONS
The pycnometer is delicate and expensive; exercise care when handling it. The bulb and
stopper of the pycnometer are both engraved with the same number. Be sure that you do
not inadvertently switch stoppers with someone else; check the numbers occasionally.
The pycnometer must be clean and DRY before the initial weighing. To fill the pycnometer
with liquid, use a Pasteur pipet to fill the bulb to about halfway up the neck (there is
usually a white mark). Then slowly insert the capillary stopper.

When full, there should be NO air bubbles in the bulb or capillary of the pycnometer, and
no air space at the top of the capillary. Before weighing the full pycnometer, the outside
should be perfectly dry.

6.3. PYCNOMETRIC METHOD

Obtain a pycnometer and glass stopper from your lab instructor. Carefully clean the
glassware with soap and water and then rinse with a small amount of acetone as
described above. Weigh the dry flask and stopper on the analytical balance. Determine
the exact volume of your pycnometer by filling it fully with water, inserting the stopper,
and tap the sides gently to remove the air bubbles. Dry the sides and weigh the filled
pycnometer on the analytical balance. Measure the temperature of the water. Use the
known density of water located in table 1 to determine the volume of water contained in
the full pycnometer flask. Be certain to use the known density value at the correct
temperature.

36
Table 1: Temperature dependence of distilled water density 𝜌𝐻2 𝑂

37
7. MEASURING THE SURFACE TENSION AND INTERFACIAL USING THE DU NOUY
RING
The Sigma tensiometer system is a modular high performance surface and interfacial
tension meter.

The surface tension measurements with the Du Nouy ring

7.1. PRE LAB ACTIVITY

To perform a measurement of surface and interfacial tension tensiometer, you must first
prepare your physical setup and software

For the best results the unit should be switched on for at least 24 hours before
measurement. Make sure your measuring vessel is thoroughly clean.

Your probe used the tensiometer should be clean with solvent and flame prior to use, the
flame source should be strong comparable to a Bunsen burner (Temperature 1000℃).

NB; low heat flames will leave residue on your probe, which will cause significant error.

Then fill your vessel with the liquid / fluid and place it on the stage. Hang the cleaned
probe on the balance hook.

To proceed with the preparation of the measurement, double click on the attension
software icon on the connected computer, to the attension software interface.

Choose surface /interfacial tension measuring icon from the connected computer. From
the software choose SI/IT button.

1. Fill in the empty field in the default recipe or open a previously stored recipe. At
least the following field should be checked

• Experiment name.

• Check that the probe dimensions are correct.

• Check that light phase is air.

• Heavy phase is the liquid you are measuring. (liquid can be choose from database
or the properties can be given manually)

2. Fill the standard beaker with the liquid you want to measure, clean the probe and
hang it on the hook. Bring the probe close to the surface to save some
measurement time and press start.

The instrument will show the measuring force/wetted length in real time and plot the
corrected surface tension values in the graph. And both measured and corrected values
will also be shown in the table format.

The instrument will make as many repeated measurements as indicated in the recipe and
stop after the measurement is completed or the stop bottom is pressed.

38
 7.2. MEASURING THE INTERFACIAL TENSION WITH THE DU NOUY RING.
PRE LAB ACTIVITY
To perform a measurement of surface and interfacial tension tensiometer, you must first
prepare your physical setup and software

For the best results the unit should be switched on for at least 24 hours before
measurement. Make sure your measuring vessel is thoroughly clean.

Your probe used the tensiometer should be clean with solvent and flame prior to use, the
flame source should be strong comparable to a Bunsen burner (Temperature 1000℃).

NB; low heat flames will leave residue on your probe, which will cause significant error.

The interfacial tension measurement is done by using the same measurement type or
method as with the surface tension measurement.

1. Fill in the empty field in the default recipe or open a previously installed recipe. At
least the following fields should be checked.

• Experiment name.

• Check that the probe dimensions are correct.

• Put the less dense liquid as light phase. (Liquid can be choose from a database or
the properties can be given manually)

• Put the more dense liquid as heavy phase. (usually water)

• Unmark the automatic surface detection.

2. Fill the standard beaker with the heavy liquid. Clean and hang the probe.

3. Lower the probe so that it is immersed in the liquid.

4. Pour the less dense liquid on top.

5. Bring the probe closer to the interface but keep it still in the heavy phase

6. Press start.

NB; the interfacial tension measurement should always be done from polar to non-polar
liquid. Most often measurement can be done as describe above since in interface tension
measurements between polar and non-polar liquids, the polar is almost always the
heavier liquid.

39
8. DETERMINATION OF VISCOSITY USING THE ROTATIONAL VISCOMETER (FANN
M35SA)
8.1. VISCOSITY TEST
The stainless steel sample cup provided has a line at the proper 350 ml test fluid level.
Fill the cup to that line with recently stirred test fluid. A scribed line on the rotor indicates
proper immersion depth. Damage to the bob shaft bearings may occur if this immersion
depth is exceeded. If other sample holders are used, the space between the bottom of the
rotor and the bottom of the sample holder should be one-half inch (1.27cm) or greater.

The viscometer is an instrument with the ability to test at six different speeds.

It ranges from 3 rpm up to 600 rpm with the speed being determined by a combination
of speed switch setting and viscometer gear knob placement. To select the desired speed,
set the speed switch located on the right side of the base to the high or low speed position
as desired. Then turn the motor on and move the viscometer gear shift knob located in
the center of the top of the instrument to its desired position.

The viscometer has twelve speed testing capabilities. To achieve this broader testing
range (from 0.9 rpm up to 600 rpm) an additional gear box shift lever is used and it is
located on the right side of the gear box. Position this lever to the Left or Right as
determined from Table 1

Table 1.0

Only the viscometer gear shift knob on the top of the instrument can be changed while
the motor is running.

40
After preparing the instrument for 12-speed testing by setting the gear box shift lever,
select the proper speed range with the speed shift switch on the right side of the base,
then turn on the motor and set the viscometer gear knob on the top of the instrument.
The stress values will appear on the dial.

8.2. MEASURING GEL STRENGTH

The commonly used procedure for measuring gel strength is as follows;

1. Stir the sample thoroughly at 600 rpm

2. Set the gear shift knob to the 3 rpm position, and then turn the motor to the OFF
position.

3. After the desired wait time, turn the motor to the ON position at low speed

4. Read the dial at the moment the gel breaks as noted by a peak dial reading.

5. The gel strength unit is lb/100ft2

An alternative method for measuring the gel strength

1. Stir the sample thoroughly at 600 rpm

2. Turn the motor to the OFF position

3. After the desired wait, turn the gel knob slowly counterclockwise

41
 4. Read the dial at the moment the gel breaks as noted by a peak dial reading.

5. The gel strength unit is lb/100ft2

8.3. NEWTONIAN VISCOSITY CALCULATIONS

Newtonian Viscosity in centipoise may be read directly from the dial when viscometer is
run at 300 rpm with R1-B1-F1 combination. Other springs may be used providing the dial
reading is multiplied by the "f" factor (spring constant).

To rapidly determine Newtonian viscosities in cP with the viscometer, use the following
formula:

𝜇𝑁 = 𝑆 × 𝜃 × 𝑓 × 𝐶

Where:

𝑆 = Speed factor (Refer to Table 3)

𝜽 = Dial reading

𝑓= spring factor (Refer to Table 4)

𝐶= Rotor-bob factor (Refer to Table 2)

𝜇𝑁 = Newtonian viscosity - cP

Example: Using an R2-B1 combination at a speed of 600 rpm with an F5.0 spring, and a
dial deflects to 189.

? N = 0.5 x 189 x 5 x .315 = 149 cP.

NOTE: Combinations with the larger gaps are likely to give results that differ from these
figures.

For best accuracy, calibrate with a standard fluid having a viscosity near the range of
interest and using the R-B-F combination to be used in the test.

42
 Table 2

Table 3

43
 Torsion Spring Torsion spring
Assembly Factor, f

F0.2 0.2

F0.5 0.5

F1 1

F2 2

F3 3

F4 4

F5 5

F10 10

Table 4

44
9. DETERMINATION OF SPECIFIC GRAVITY USING API HYDROMETER METHOD
The API hydrometer is used to determine oil gravity in the oil field. When a hydrometer is
placed in oil, it will float with its axis vertical after it has displaced a mass of oil equal to the
mass of the hydrometer. The hydrometer can be used at atmospheric pressure or at any other
pressure in a pressure cylinder.

API gravity is a special function of specific gravity at 15℃ (60℉) and is represented by
141.5
𝐴𝑃𝐼 𝑔𝑟𝑎𝑣𝑖𝑡𝑦, 𝑑𝑒𝑔𝑟𝑒𝑒 =𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑔𝑟𝑎𝑣𝑖𝑡𝑦 𝑎𝑡 15℃ −131.5

Accurate determination of density, specific gravity and API gravity of petroleum is important
for the conversion of measured volumes to volumes at the standard temperature of 15℃ or
60℉. Density and specific gravity especially API gravity is a governing factor for the quality
and crude pricing are always posted against API values.

Figure 1.0; Hydrometer.

Apparatus; Hydrometer, Measuring cylinder, sample, thermometer, stirring rod, hot water
bath, filter paper

9.1. PROCEDURE;
1. Prepare a sample and place it in the water bath till its temperature is 15℃ and heat
the hydrometer cylinder to approximately the same temperature as the sample to be
tested.

2. Transfer the sample to the hydrometer cylinder without splashing to avoid the
formation of air bubbles and reduce to a minimum the evaporation of the lower point
constituents. Remove any air bubbles formed, after they have collected on the surface
of the sample by touching them with a filter paper.

3. Lower the hydrometer gently into the sample. Take care to avoid wetting the stem
above the level to which it will be immersed. Continuously stir the sample. With a
thermometer record the temperature of the sample and remove the thermometer.

4. Depress the hydrometer about two scale divisions into the liquid and then release it.
The remainder of the stem of the hydrometer, which is above the level of the liquid,
must be kept dry.

5. When the hydrometer comes to rest estimate the hydrometer scale reading. The
correct hydrometer reading is that point on the hydrometer scale at which the surface
of the liquid cuts the scale. Determine this point by placing the eye slightly below the
level of the liquid and slowly raising it until the surface, first seen as a distorted ellipse,
appears to become a straight line cutting the hydrometer scale.

45
 6. Immediately after observing the hydrometer scale value, stir the sample with a
thermometer. Take the thermometer reading. If this is different from the first reading
take the hydrometer measurement again till the temperature becomes constant. The
reading you will obtain is the hydrometer reading at a given temperature.

9.2. CALCULATION
Convert the reading using the provided tables.

Calculate the density, specific gravity and API gravity.

46
10. LIQUID VISCOSITY MEASUREMENT USING CAPILLARY TYPE VISCOMETER
10.1. DESCRIPTION:
The main objective of the measurement is to determine the kinematic viscosity of Newtonian
liquid petroleum products.

For capillary viscometers the time is measured in seconds for a fixed volume of liquid to flow
under gravity through the capillary at a closely controlled temperature. The kinematic
viscosity is the product of the measured flow time and the calibration constant of the
viscometer. The dynamic viscosity can be obtained by multiplying the measured kinematic
viscosity by the density of the liquid.

10.2. DEFINITIONS
Dynamic viscosity (μ) is the ratio between the applied shear stress and the rate of shear and
is called coefficient of dynamic viscosity μ. This coefficient is thus a measure of the resistance
to flow of the liquid; it is commonly called the viscosity of the liquid.

Kinematic viscosity (υ) is the ratio μ/ρ where ρ is fluid density.

10.3. PROCEDURE:
1. Select a clean, dry calibrated viscometer (Fig. 4.6) having a range covering the
estimated viscosity (i.e. a wide capillary for a very viscous liquid and a narrower
capillary for a less viscous liquid). The flow time should not be less than 200 seconds.

2. Charge the viscometer: To fill, turn viscometer upside down. Dip tube (2) into the
liquid to be measured while applying suction to tube (1) until liquid reaches mark (8).
After inverting to normal measuring position, close tube (1) before liquid reach mark
(3).

3. Allow the charged viscometer to remain long enough to reach the room temperature.
Read the calibration constants-directly from the viscometer.

4. Measuring operation: Open tube (1) and measure the time it takes the liquid to rise
from mark (3) to mark (5). Measuring the time for rising from mark (5) to mark (7)
allows viscosity measurement to be repeated to check the first measurement.

5. If two measurements agree within required error (generally 0.2-0.35%), use the
average for calculating the reported kinematic viscosity.

47
 Figure 1.1 Canon Fenske viscometer

10.4. CALCULATION AND REPORT:

1. Calculate the kinematic viscosity υ from the measured flow time t and the instrument
constant by means of the following equation:

υ = C(t −ϑ )

Where:

υ = kinematic viscosity, cSt

C = calibration constant, cSt/s

t = flow time, s

ϑ = Hagenbach correction factor, when t < 400 seconds, it should be corrected according to
the manual. When t > 400 seconds, ϑ = 0.

2. Calculate the viscosity μ from the calculated kinematic viscosity υ and the density ρ by
means of the following equation:

μ = ρ avr υ

Where:

μ = dynamic viscosity, cp

ρavr = average density in g/cm3 at the same temperature used for measuring the flow
time t.

υ = kinematic, cSt.

3. Report test results for both the kinematic and dynamic viscosity. Calculate the average
dynamic viscosity.

48
49
 DRILLING
FLUIDS
AND
WELL
CEMENTING
LAB
50
11. MUD WEIGHT, MARSH FUNNEL VISCOSITY AND pH
11.1. MUD WEIGHT OR DENSITY TEST
Theory
This test procedure is a method for determining the mass of a given volume of liquid which is
equivalent to density. Mud weight controls hydrostatic pressure in a wellbore and prevents
unwanted flow into the well. The weight of the mud also prevents collapse of casing and the
openhole. Excessive mud weight can cause lost circulation by propagating, and then filing, fractures
in the rock. Therefore the density of the drilling fluid must be controlled to provide adequate
hydrostatic head to prevent influx of formation fluids, but not so high as to cause loss of circulation
or adversely affect the drilling rate and damaging the formation.
Normal pressure gradient by water is equal to (0.433 psi/ft) and equal to 433 psi/1000 ft.

Test Equipment- using the Fann Mud Balance: Model 140 Mud Balance
The Mud Balance as shown below is used to determine density of the drilling fluid. The instrument
consists of a constant volume cup with a lever arm and rider calibrated to read directly the density
of the fluid. The four (4) calibrated scales on the mud balance allow the drilling fluid density to be
read directly in units of Pounds per gallon (LBS/Gal. Also known as ppg), Pounds per Cubic feet
(LBS/cu.ft), Grams per cubic centimetre (g/𝑐𝑚 3 . 𝐴𝑙𝑠𝑜 𝑐𝑎𝑙𝑙𝑒𝑑 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑔𝑟𝑎𝑣𝑖𝑡𝑦 𝑜𝑟 𝑆𝐺) or as a drilling
fluid pressure gradient in Pounds per square inch per 1000 feet (LBS/SQ.IN./1000ft or psi/1000ft).

Figure 1.1: Typical Mud Balance

11.2. CALIBRATION
1. Remove the lid from the cup, and completely fill the cup with water.
2. Replace the lid and wipe dry.
3. Replace the balance arm on the base with knife-edge resting on the fulcrum.
4. The level vial should be centered when the rider is set on 8.33. If not, add to or remove shot
from the well in the end of the bream.

11.3. TEST PROCEDURE

1. Remove the lid from the cup, and completely fill the cup with the mud to be tested.
2. Replace the lid and rotate until firmly seated, making sure some mud is expelled through the
hole in the cup.
3. Wash or wipe the mud from the outside of the cup.
4. Place the balance arm on the base, with the knife-edge resting on the fulcrum.
5. Move the rider until the graduated arm is level, as indicated by the level vial on the beam.
6. At the left-hand edge of the rider, read the density on either side of the lever in all desired
units without disturbing the rider.
7. Note down mud temperature corresponding to density.

51
 11.4. MARSH FUNNEL VISCOSITY:
THEORY
The viscosity of a fluid is defined as its resistance to flow. The desired viscosity for a particular
drilling operation is influenced by several factors, including mud density, hole size, pumping rate,
drilling rate, pressure system and requirements, and hold problems. The indicated viscosity as
obtained by any instrument is valid only for that rate of shear and will differ to some degree when
measured at a different rate of shear.
For field measurements the marsh funnel has become the standard instrument.

TEST EQUIPMENT
The Marsh Funnel is a device that is common to every drilling rig. Figure 1.2 shows an image of the
Marsh Funnel and receiving cup. The viscosity is reported in seconds allowed to flow out of the
funnel. API specifications call for 1500 ml and one quart (946) ml out.
For API water at 70 F + 0.5oF = 26 + 0.5 sec. The Marsh Funnel measures the apparent viscosity.

Figure 1.2: Marsh Funnel and One-liter Cup

CALIBRATION
Fill the funnel to the bottom of the screen (1500 ml) with water at 70 F (plus or minus 0.5 F) time of
outflow of the quart (946 ml) should be 26 seconds plus or minus 1/2 second.

TEST PROCEDURE
1. With the funnel in an upright position, cover the orifice with a finger and pour the freshly
collected mud sample through the screen into a clean, dry funnel until the fluid level reaches
the bottom of the screen (1500 ml).
2. Immediately remove the finger from the outlet and measure the time required for the mud to
fill the receiving vessel to the 1-quart (946 ml) level.
3. Report the result to the nearest second as Marsh Funnel Viscosity at the temperature of the
measurement in degrees Fahrenheit or Centigrade.

11.5. HYDROGEN ION CONCENTRATION (PH)

THEORY
The acidity and the alkalinity of the drilling fluid can be measured by the concentration of the H + ion
in the fluid. As for instance, if H+ is large (1 x 10-1), then the OH- hydroxyl concentration is very low
(1 x 10-13), the solution is strongly acidic. If the (OH-) concentration is (1 x 10-1) very high then (H+)
concentration is very low then the solution is strongly alkaline. The pH of a solution is the logarithm
of the reciprocal of the (H+) concentration in grams moles per liter, expresses as:
1
𝑝𝐻 = 𝑙𝑜 𝑔 { } = − log 𝐻 +
𝐻+
Example: If the solution is neutral then H+ and OH- concentrations are the same equal to 1 x 10 -7.
52
 1
𝑝𝐻 = log ( ) = − log[1 𝑥 10−7 ] = − [−7] = 7.00
1 𝑥 10−7
Therefore, if the pH of a mixture drops from 7.0 to 6.0, the number of (H +) increase ten times.

The pH of a mud seldom is below 7 and in most cases fall between 8 and 12.5 depending upon the
type of mud. The pH is important because the pH affects the solubility of the organic thinners and
the dispersion of clays presents in the mud.

METHODS OF MEASURING PH IN THE LABORATORY

1. The pH Paper: The pH paper strips have dyes absorbed into the paper display certain colors
in certain pH ranges. It is useful, inexpensive method to determine pH in fresh water muds.
The main disadvantage is that high concentrations of salts (10,000 ppm chloride) will alter
the color change and cause inaccuracy.
2. The pH Meter: The pH meter is an electric device utilizing glass electrodes to measure a
potential difference and indicate directly by dial reading the pH of the sample. The pH meter
is the most accurate method of measuring pH.

Figure 1.4: pH Meter

LABORATORY EXPERIMENT
1. Take 2 samples of drilling mud
2. Stir the samples for 2 minutes and determine:
a. The Mud Weight
b. Marsh Funnel Viscosity in seconds
c. pH value using
i. pH meter
ii. Hydrion papers / pH paper

53
Tabulate your results in the following format:

Room temperature: oF/ oC

Sample No. Mud Weight Marsh pH (hydrogen ion

Funnel concentration)
viscosit
y
LBS/Gal LBS/Cu.ft g/𝑐𝑚 3 LBS/SQ.IN./1000f seconds pHydrion pH meter
SG t
1

11.6. QUESTIONS
Answer the following:

1. List any five (5) very important functions of the drilling fluid?
2. What requirements should a drilling fluid meet?
3. Using the mud weights (ppg) obtained for Samples #1 and 2 of your experiment, calculate,
how much hydrostatic pressure that each sample will exert on a formation at a depth of
10,000 ft.
4. What is the difference between Over-balance and Under-balance?
5. Estimate the mud weight needed to balance a formation pressure equivalent to 10,000 ft.
depth with 0.561 psi/ft. pressure gradient.

54
12. MUD RHEOLOGY TEST
12.1. INTRODUCTION
Rheology refers to the deformation and flow behavior of all forms of matter. Certain rheologic
measurements made on fluids, such as viscosity, gel strength, etc. help determine how this fluid will
flow under a variety of different conditions. This information is important in the design of circulating
systems required to accomplish certain desired objectives in drilling operations.

12.2. VISCOSITY
THEORY
Viscosity is defined as the resistance of a fluid to flow and is measured as the ratio of the shearing
stress to the rate of shearing strain.

Two types of fluid characterizations are:

1. Newtonian (true fluids) where the ratio of shear stress to shear rate or viscosity is constant,
e.g. water, light oils, etc. and
2. Non-Newtonian (plastic fluids) where the viscosity is not constant, e.g. drilling muds,
colloids, etc.

Figure 2.1: Flow Curves of Newtonian and non-Newtonian Fluids

TEST EQUIPMENT
The Fann (Model 286) Rheometer is a coaxial cylindrical rotational viscometer, used to determine
single or multi-point viscosities. It has fixed speeds of 3 (GEL), 100, 200, 300 and 600 RPM that are
switch selectable with the RPM knob. Additionally, the same switch set to the VAR position enables
speed selection of between 3 and 625 RPM, by manual adjustment of the variable knob.

55
Figure 2.2: Variable Speed Rheometer

TEST PROCEDURE
1. Fill the cup with a recently agitated sample to the scribe line. Tilt back the upper housing of
the rheometer, locate the cup under the sleeve (the pins on the bottom of the cup fit into the
holes in the base plate), and lower the upper housing to its normal position.
2. Turn the knurled knob between the rear support posts to raise or lower the rotor sleeve
until it is immersed in the sample to the scribe line.
3. Stir the sample for about 5 seconds at 600 RPM, then select the RPM desired speed for the
test.
4. Wait for the dial reading to stabilize (the time depends on the sample's characteristics).
5. Record the dial reading and RPM.

RHEOLOGICAL CALCULATIONS
Plastic viscosity (in centipoise, cp):

𝑃𝑙𝑎𝑠𝑡𝑖𝑐 𝑉𝑖𝑠𝑐𝑜𝑠𝑖𝑡𝑦 = µ𝑝 = 600 𝑅𝑃𝑀 𝑟𝑒𝑎𝑑𝑖𝑛𝑔 − 300 𝑅𝑃𝑀 𝑅𝑒𝑎𝑑𝑖𝑛𝑔

Apparent Viscosity (in centipoise, cp):

600 𝑅𝑃𝑀 𝑅𝑒𝑎𝑑𝑖𝑛𝑔
𝐴𝑝𝑝𝑎𝑟𝑒𝑛𝑡 𝑉𝑖𝑠𝑐𝑜𝑠𝑖𝑡𝑦 = µ𝑎 =
2
Yield Point (in lb/100ft2):

𝑌𝑖𝑒𝑙𝑑 𝑃𝑜𝑖𝑛𝑡 = 𝑌. 𝑃. = 300 𝑅𝑃𝑀 𝑅𝑒𝑎𝑑𝑖𝑛𝑔 − 𝑃𝑙𝑎𝑠𝑡𝑖𝑐 𝑉𝑖𝑠𝑐𝑜𝑠𝑖𝑡𝑦

12.3. GEL STRENGTH:

THEORY
The Fann Rheometer is also used to determine the Gel strength, in lb/100 sq. ft., of a mud. The Gel
strength is a function of the inter-particle forces. An initial 10-second gel and a 10-minute gel
strength measurement give an indication of the amount of gelation that will occur after circulation
ceased and the mud remains static. The more the mud gels during shutdown periods, the more
pump pressure will be required to initiate circulation again.

Most drilling muds are either colloids or emulsions which behave as plastic or non-Newtonian fluids.
The flow characteristics of these differ from those of Newtonian fluids (i.e. water, light oils, etc.) in
that their viscosity is not constant but varied with the rate of shear, as shown in Figure 2.1.
Therefore, the viscosity of plastic fluid will depend on the rate of shear at which the measurements
were taken.

TEST PROCEDURES
1. Stir a sample at 600 RPM for about 15 seconds.
2. Turn the RPM knob to the STOP position.
3. Wait the desired rest time (normally 10 seconds or 10 minutes).
4. Switch the RPM knob to the GEL position.
5. Record the maximum deflection of the dial before the Gel breaks, as the Gel strength in
lb/100 ft2.

NB: (lb/100 ft2 x 5.077 = Gel strength in dynes/cm2).

56
 12.4. YIELD POINT
THEORY
This is the measure of the electro-chemical or attractive forces in the mud under flow (dynamic)
conditions. These forces depend on:
• surface properties of the mud solids,
• volume concentrations of the solids and
• electrical environment of the solids.
The yield point of the mud reflects its ability to carry drilled cuttings out of the hole.

CALCULATION:
𝑌𝑖𝑒𝑙𝑑 𝑃𝑜𝑖𝑛𝑡 = 300 𝑅𝑃𝑀 − 𝑃𝑙𝑎𝑠𝑡𝑖𝑐 𝑉𝑖𝑠𝑐𝑜𝑠𝑖𝑡𝑦

EXPERIMENT
1. Obtain 2 recently agitated mud
2. Using the Baroid Rheometer, obtain dial readings at 3, 300 and 600 RPM.
3. By means of the rheological calculations procedure, determine the Apparent and Plastic
Viscosities, Yield Point and initial 10 sec. and final 10-minute Gel Strength parameters.
4. Tabulate your results as in the given table below:

MUD RHEOLOGY TEST WATER BASE MUD

Sample Viscosity, cP Gel Strength, lb/100ft2

No.
ɸ600 ɸ300 µp µa Yp Initial 10 sec Final 10 min.
lb/100ft2 gel gel

12.5. QUESTIONS
1. (a)What is Plastic Viscosity?
(b) What does it characterize?
(c)What is the difference between the Plastic Viscosity and Apparent viscosity of a drilling
fluid?
2. Which role does Gel Strength play in the drilling process?
3. What type of fluids does drilling fluid belong to?
4. (a) What is the Yield Point?
(b) What does it characterize?
(c)What is the difference between Gel Strength and Yield Point of a drilling mud?
5. Explain what you know about one point and two points curve fluids? Give one example of
each type of fluid.

57
13. FILTRATION, WALL BUILDING, AND RESISTIVITY
13.1. FILTRATION THEORY
The loss of liquid from a mud due to filtration is controlled by the filter cake formed of the solid
constituents in the drilling fluid. The test in the laboratory consists of measuring the volume of liquid
forced through the mud cake into the formation drilled in a 30 minute period under given pressure
and temperature using a standard size cell.

It has been found in early work that the volume of fluid lost is roughly proportional to the square
root of the time for filtration, i.e.

𝑉 ∝ √𝑡

The two commonly determined filtration rates are the low-pressure, low-temperature and the high-
pressure high-temperature.

13.2. TEST EQUIPMENT

The low pressure test is made using standard cell under the API condition of 100 ± 5 psi for 30
minutes at room temperature. Another special cell, the HPHT filter press can be used to measure
filtration rate at elevated temperatures and pressure.

The OFITE filter press used for filtration tests consists of six independent filter cells mounted on a
common frame. Each cell has its own valve such that any or all the cells could be operational at the
same time. Toggle valve on the top of each cell could be operated independently for the supply of air
for each individual cell.

Special high pressure and high temperature filtration tests are run in the laboratory simulating
formation temperature and formation back- pressure.

Fig 3.1: Standard API Filter Press

58
Fig 3.2: High Temperature High Pressure Filter Press

13.3. TEST PROCEDURE FOR FILTRATION RATE AT 100 PSI & ROOM
TEMPERATURE
1. Assemble the test cell in this order: Base cup, Rubber gasket, Screen, Sheet of filter paper,
Rubber gasket and Cell body
2. Fill the cell with test sample to within 0.5" of the top.
3. Place the rubber gasket in place in the top cup and set it on the cell and mount this unit in the
frame. Secure the cell with T-screw.
4. Place a dry graduated cylinder under the filter tube.
5. Attach a regulated pressure source to the inlet port of the pressure manifold and apply 100
PSI pressure to the filter cell by opening the valve above the cell(s) to be tested. The time of
test begins at that moment.
6. At the end of 1, 4, 7.5, 9, 16, 25, 30, and 36 minutes, measure the volume of filtrate and
record it.
7. After that close the valve of nitrogen cylinder and open the safety bleeder valve. This will
release the pressure of the entire system.

13.4. WALL BUILD

MEASUREMENT PROCEDURE FOR MUD CAKE THICKNESS
After the filtration process described above, disassemble the cell and remove the filter paper from
the cup. The mud cake is deposited on filter paper. Wash excess off the mud from the cake gently
with water and measure its thickness.

It should be reported in thirty-second of an inch in whole number. Vernier caliper could be used to
measure the thickness, however, while measuring care should be taken not to press vernier jaw on
mud cake to penetrate through.

Results on mud cake thickness should be reported in whole number.

Example: 0.75/32" should be reported as 1/32. I.e. closest to the whole number.
Likewise 1.75/32" should be reported as 2/32"

13.5. MUD RESISTIVITY

THEORY
The resistivity (Wm) of a drilling mud is influenced by the dissolved salts (ppm) or (gpg, grain per
gallon) in the water portion and the insoluble solid material contained in the water portion. The
greater the concentration of dissolved salts, the lower resistivity of the solution. Unlike metals, the
resistivity of a solution decreases as temperature increases. It is necessary to measure resistivity
because the mud, mud cake, mud filtrate resistivity exert a strong effect on the electric logs taken in
59
that mud. The mud resistivity varies greatly from the actual resistivity values due to the various
factors encountered in the actual operation.

Test Equipment

Equipment used is the OFITE Resistivity Meter (Fig. 3.3).

Figure 3.3: Digital Resistivity Meter

Upon turning on the resistivity meter, the display screen will show the temperature and either
Resistivity or Concentration of NaCl. To change the measurement reading, press the “Menu” button,
then press the “Units” button to toggle between Resistivity and Concentration of NaCl. Press the
“Select” button to save your choice.

To change the units, press the “Units” key repeatedly until you reach the desired units. Press the
“Select” button to save your choice. The “Units” button offers the following options:

a. Degrees C
b. Degrees F
c. Concentration in Parts Per Million (ppm)
d. Concentration in Kilo Parts Per Million (kppm)
e. Concentration in Grains Per Gallon (gr/gal)

13.6. MEASUREMENT PROCEDURE FOR MUD CAKE RESISTIVITY

1. Remove excess water from filter cake.
2. Fill the slot on top of the cell with mud cake. Be sure the sample fills the area between the
two metal posts in the cell.
3. Connect the cell to the two terminal posts on the meter. Wait for the sample to reach room
temperature.
4. Reading on the meter is the resistivity of mud cake.
5. Record the resistivity of the mud cake and the temperature of the cell.
6. Remove the cell and clean thoroughly with distilled water.

13.7. MEASUREMENT PROCEDURE FOR MUD FILTRATE RESISTIVITY

1. Use the suction bulb to pull the sample into the lucite cell. Empty and refill the cell several
times to thoroughly wet the cylinder walls.
2. Connect the cell to the two terminal posts on the meter. Be sure the sample fills the area
between the two metal posts in the cell.
3. Wait for the sample to reach room temperature.
The reading on the meter is the resistivity of the mud (when testing mud it may be necessary
to allow 3-5 minutes after putting mud in the cell before taking a reading to allow cell and
the mud filtrate to reach temperature equilibrium).
4. Record the resistivity reading and the temperature of the cell.

60
 13.8. QUESTIONS
1. Describe how the filter cake is formed on the walls of a hole during a normal drilling
operation.
2. What are the factors controlling the rate of filtration?
3. What is sloughing of shale and how can it be controlled?

14. CONTROL OF MUD WEIGHT

14.1. EFFECT OF ADDING WEIGHT MATERIAL (BARITE)
THEORY
Barite was first used, in California, in a well being re-drilled with cable tools in 1923. According to
that case, density of the mud was raised to 90 lb/ft3 (1.44 g/cm 3) to control gas in flow and to stop
caving.

One function of barite has developed - the preparation of a temporary high-density plug formed
from slurry of a barite in water (2.65 S.G). Such slurry contains the maximum concentration of barite
that is used -about 750 lb/bbl (2100 kg/cm3). The minimum concentration of barite might be as low
as 10 lb/bbl (28 kg/m3), although usually it would be substantially higher.

The quantity of barite required to raise the density of a given volume of mud a specific amount can
be readily calculated from the relation, in consistent units:

𝑉𝑜 𝜌𝑜 + 𝑉𝐵 𝜌𝐵 4.3 ∗ 𝑉𝑜 (𝜌𝑓 − 𝜌0 )
𝜌𝑓 = ⇒ 𝑊𝑡𝐵 =
𝑉𝑜 + 𝑉𝐵 𝜌𝐵 − 𝜌𝑓

Where:

𝜌𝑓 = 𝐹𝑖𝑛𝑎𝑙 𝑚𝑢𝑑 𝑑𝑒𝑛𝑠𝑖𝑡𝑦

𝜌𝑜 = 𝑂𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑚𝑢𝑑 𝑑𝑒𝑛𝑠𝑖𝑡𝑦

𝜌𝐵 = 𝐵𝑎𝑟𝑖𝑡𝑒 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 = 35.82 ppg

𝑉𝑜 = 𝑂𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑚𝑢𝑑 𝑣𝑜𝑙𝑢𝑚𝑒

𝑉𝐵 = 𝐵𝑎𝑟𝑖𝑡𝑒 𝑣𝑜𝑙𝑢𝑚𝑒

𝑊𝑡𝐵 = 𝐵𝑎𝑟𝑖𝑡𝑒 𝑤𝑒𝑖𝑔ℎ𝑡

NB: Specific gravity of Barite = 4.3

TEST PROCEDURE
1. Calculate and list the amount of barite required to increase the density of each batch from
8.6 ppg to 9, 10, 11 and 12 ppg.
2. Obtain 400 cc of original base mud (density 8.6)
3. Add the calculated amount of barite to each batch, stir for about 2 minutes and measure the
Apparent and Plastic Viscosities and Yield Point.
4. Repeat step 3 for Salt water-base mud.
5. Tabulate the results and plot the density (ppg ), viscosity (apparent and plastic) and yield
point versus the amount of barite added.

61
 14.2. EFFECT OF ADDING BENTONITE ON MUD PROPERTIES FOR FRESH AND
SALT WATER BASE MUD:
PROCEDURE
1. Add to every 400 cc batch of fresh water base mud 2, 4, 6 and 8 grams of bentonite and stir
for 10 minutes.
2. Measure the density in lb/gal, viscosity (apparent and plastic) and yield point in lb/100 ft,
using the Rheometer for every batch.
3. Add 20.6 ml of 10% by weight salt water to every batch. Stir for 5 minutes and repeat step
(2).
4. Report all the results (density, viscosities, and yield) for every batch in a convenient table.
Plot them versus the amount of bentonite in gram in two plots, one for fresh water and the
other for salt water.

14.3. WATER-BACK (ADDING WATER TO A CHEMICALLY TREATED MUD)

1. Obtain a 350 c.c. of water base mud of 13.5 ppg weight and 9.5 pH.
2. Add water incrementally and measure the Mud weight every time to reach 10.5 ppg and
same (9.5) pH.
3. Measure the viscosity and gel-strength and check if any change occurred.
4. List your results in an appropriate table.

14.4. QUESTIONS
1. List the advantages obtained by adding weighting material to mud.
2. List three (3) names of weighting material.
3. What are the disadvantages of adding solids to the water based mud?
4. Give reasons for adding water to your mud.

Include the following points in your discussions:

• Discuss the effect of adding bentonite on density.

• Discuss the effect of adding bentonite on the rheological properties.
• Correlate and justify the results obtained for fresh and salt water.

What is the effect on yield point?

62
15. SOLID & LIQUID CONTENT AND EMULSION CHARACTERISTICS OF DRILLING
FLUID
15.1. SAND CONTENT DETERMINATION
THEORY
Periodic sand content determination of drilling mud is desirable, because excessive sand may result
in the deposition of a thick filter cake on the wall of the hole, or may settle in the hole about the tools
when circulation is stopped, thus interfering with successful operation of drilling tools or setting of
casting. High sand content also may cause excessive abrasion of pump parts and pipe connections.

Sand content is determined by elutriation, settling, or sieve analysis. Of the three methods, sieve
analysis is preferred because of reliability of test and simplicity of equipment. The volume of sand,
including void spaces between grains, is usually measured and expressed as percentage by volume
of the mud.

TEST EQUIPMENT:
The Sand Content Set consists of a 200-mesh sieve, funnel, and a glass measuring tube calibrated
from 0 to 20% to read directly the percentage sand by volume.

Figure 6.1: Sand Content Set

TEST PROCEDURE
1. Pour mud into the Sand Content Tube until it fills up to the mark labeled "Mud to Here". Then
add water to the mark labeled "Water to Here". Cover mouth of the tube with thumb and
shake vigorously.
2. Pour this mixture through the screen, being careful to wash everything out of the tube with
clear water through the same screen. Wash sand retained on screen with a stream of water
to remove all mud and shale particles.
3. Fit funnel down over top of screen, invert slowly turning tip of funnel into mouth of tube, and
wash sand back into tube with a fine spray of clear water on the back side of the screen.
Allow the sand to settle.
4. Observe the quantity of sand settled in the calibrated tube as the sand content of the mud.

Report the sand content of the mud in percent by volume (% by volume). Take into account coarse
solids obtained on the screen.

NB:

63
 • In step 2 of the procedure, the pouring of the mud and water mixture through the screen can
be facilitated by tapping the side of the screen with a spatula handle.
• Contents retained on the screen in Step 2 of the procedure should not be mashed, stirred, or
mutually forced through the screen with a finger, pencil, or the like, as this will give an
erroneous reading and may pull the screen loose from the side of the container.

15.2. EMULSION TEST

THEORY
Emulsion testers are used to indicate the stability and type of emulsion whether water-in-oil or oil-
in-water. They are used in the evaluation of inverted emulsion drilling fluids, cements, and
fracturing fluids. Time stability and resistance to electrolyte contamination of these systems can be
predicted from a measurement of relative emulsion stability.

Test Equipment

Figure 6.2: Ofite Emulsion stability meter

TEST PROCEDURE
1. Pre-heat the oil mud sample to 120°F (48.8°C).
2. Pour the sample through a 12-mesh screen or Marsh Funnel screen into a glass or plastic
container. Do not use a metal container. Record the mud temperature
3. Hand stir the sample with the electrode probe for approximately 10 seconds. This will help
create a uniform composition and temperature. Position the electrode probe so that it does
not touch the bottom or sides of the container. Be sure the electrode surfaces are completely
covered by the sample.
4. Push the button to begin the voltage ramp. Do not move the electrode during the voltage
ramp.
5. At the conclusion of the ramp test, note the ES value displayed on the readout.
6. Repeat the above procedure with the same mud sample. The two ES values should not differ
by more than 5%. If they differ by more than 5%, the meter or electrode should be checked.
7. Record the average of the two ES measurements

15.3. OIL, WATER, SOLID & CLAY CONTENT DETERMINATION:

THEORY
Knowledge of the liquid and solids content of a drilling mud is essential for good control of the mud
properties. Such information will often explain poor performance of the mud and indicate whether
the mud can best be conditioned by the addition of water or whether treatment with chemical
thinner or the removal of the contaminant is required. Similarly, proper control of an oil emulsion
mud depends upon a knowledge of the oil content.
64
For muds containing only water and solids, the quantity of each can be determined from the mud
density and from the evaporation of a weighed sample of mud. Oil and water content can also be
obtained measuring the liquid fraction. The latter method is only applicable to oil emulsion muds.

TEST EQUIPMENT
The apparatus required to determine the oil, water and solids content of the mud is included in the
The Ofite Oil and Water Retort Kit

Figure 6.3: Oil/Water Retort Kit

TEST PROCEDURE
1. Lift retort assembly, out of insulator block. Using the spatula as a screwdriver, remove the
mud chamber from the retort.
2. Pack the upper chamber with very fine steel wool.
3. Fill mud chamber with mud and replace lid, allowing excess to escape. (This is a point where
error is often introduced. Be sure that no air is trapped in the chamber. An accurate charge of
mud is essential).
4. Wipe off excess mud and screw mud chamber into upper chamber.
5. Replace retort in insulator block and put insulation cover in place.
6. Place a clean, dry liquid receiver under the condenser discharge tube
7. Connect the retort to an electrical outlet to turn it on. Observe the liquid exiting the
condenser. Continue heating for ten minutes beyond the time that no more condensate is
being collected. (If whole mud boils over into the receiver tube, the test must be rerun. Pack
the retort body with a larger amount of steel wool and rerun the test. Allow it to run a
minimum of 45 minutes.) The light on the front of the retort will turn on while the heaters
are engaged.
8. Remove the liquid receiver and allow it to cool. After it has cooled to ambient temperature,
read and record the volumes (or volume percentage) of the following:
a. total liquid volume
b. oil volume
c. water volume

NB:

Nearly 100% recovery of refined oil will be obtained with this retort. If the mud is made up with
crude oil, calibration runs should be made on mud containing a known percentage of the crude used.
Recovery on some crudes may be as low as 60%. If the distillation is being carried on for more than
30 minutes, the retort should be removed occasionally in the uncontrolled units and observed for
temperature. In any case, the retort should never be heated above a DULL RED HEAT. The heater
will burn out is left on too long.
65
 15.4. THEORY AND CALCULATIONS OF SOLID CONTENT
The solid phase of a drilling mud units of two components, i.e.

• High specific gravity solids with a specific gravity of 4.3

• Low specific gravity solids with a specific gravity of 2.5.

The total solids phase, in volume %, is found by the Oil and Water Retort.

The information (data) from the retort test can be used to calculate the average specific gravity of
solids, the % of different types of solids, and the % solids by weight in the mud, as shown below:

NOTE: The accuracy of your calculations depends on the retort test data. These care should be taken
while running the equipment to ensure good results.

Calculations
A ⇒ % oil by volume = ml oil x 10

B ⇒ % water by volume = ml water x 10

C ⇒ % solids by volume = 100 - (ml oil + ml water) x 10

*D ⇒ Grams oil = corrected ml oil x 0.8

E ⇒ Grams water = ml water

F ⇒ Grams mud = lb/gal mud weight x 1.2

G ⇒ Grams solids = F - (D + E)

H ⇒ ml solids = 10 - (ml oil + ml water)

𝐺
I ⇒ Average specific gravity of solids = 𝐻

𝐺
J ⇒ Solids % by weight = 𝐹 𝑥 100

K ⇒ High gravity (4.3) solids % by volume = (I - 2.5) x 55.6

L-Low gravity (2.5) solids % by volume = 100 - K

* Corrected ml of oil = ml of oil

Table 6.1: Specific Gravity and Percent by Weight of Mud Contents

Sp. Gr. of Solids 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.3

% by Weight Barite 0 18 34 48 60 71 81 89 100

% by Weight Clay 100 82 66 52 40 29 19 11 0

Presentation of Experimental Results

1. Using your calculated results of the average specific gravity of solids, determine the solid
content of each of the samples from Table 6.1 (either directly or by interpolation, whichever
is applicable).
2. Present the results of your findings in (1) in an appropriate table.
66
15.5. QUESTIONS
1. From the results of your experiment in part (A), is there a correlation between the mud
weight of the sample and the % sand by volume? Explain.
2. What problems are you likely to encounter during drilling operations if you have a high sand
content in your drilling mud?
3. What is the importance of conducting Emulsion Stability tests on drilling fluids?
4. From the results of your experiment in part (C), which of the samples has the highest clay
content?

67
16. OIL WELL CEMENTING EXPERIMENT
16.1. WATER RATIOS FOR PORTLAND CEMENT SLURRY
OBJECTIVE
To show the effects of varying amounts of mixing water on the physical properties of Portland cement.
These properties are Free Water Separation, Normal and Minimum Water Content and Thickening
Time.

TEST EQUIPMENT
The Atmospheric Consistometer consists of a Stainless Steel Water bath that houses the slurry
containers. An instrument panel houses components that allow control of the bath at any temperature
from ambient to 93oC, and rotation of the slurry containers at 150 RPM. Units of consistency of the
cement are directly indicated on the top dials of the slurry containers. The containers are rotated by
engaging the pins of the lid in the slots of the rotator. The rotators have timing sprockets, belt driven
by a gear-head motor. The belt also drives an impeller, which agitates the bath water. The motor
should be turned off while engaging or disengaging the containers. Temperature is indicated and
controlled by a Thermocouple actuated Potentiometric Type Temperature Controller. The Controller
actuates a relay, controlling a 1,500- watt heater. Switches and Pilot Lights are provided as required
by the operation. A dial thermometer indicates bath temperature when the temperature controller
indicator is off the scale. The entire instrument has overall dimensions of 15" (39 cm) wide x 15" (38
cm) deep x 19" (48 cm) high.

Fig. 7.1: Atmospheric Consistometer Fig. 7.2 Pressurized Consistometer

16.2. FREE WATER SEPARATION TEST PROCEDURE

1. Weight out 400 grams of cement into each of three quart jars. The dry cement sample should
be passed through the sieve in order to remove lumps and foreign materials. The cement
temperature should be about 80oF.
2. Prepare 170 cc, 190 cc and 210 cc of sweet water into three 250 graduate cylinders. This
amount of water will produce cement slurries with water to cement ratio of 0.425, 0.574,
and 0.525 by weight.

68
 3. Add the cement samples to the three water volumes in a metal quarts while the mixer was on
low speed. When all cement has been added, turn the blender to high speed, and mix the
slurry for 35 seconds.
4. Pour 225 c.c. of slurry into 250 c.c. graduated cylinder. Tightly cover them with aluminium
foil. Allow to stand for two hours.
5. Carefully decant the free water and measure in a 10 c.c. graduated cylinder. Do this for each
slurry. Calculate the per cent (%) free water upon settling.

16.3. NORMAL & MINIMUM WATER CONTENT OF CEMENT SLURRY:

TEST PROCEDURE
1. Prepare 4 slurry samples of varying water to cement ratios, as described in part (A) 1 & 2.
2. Pour the samples immediately into an Atmospheric Consistometer and stir for a period of 20
minutes, under ambient conditions.
3. Record the Consistency immediately after 20 minutes of stirring has elapsed.
4. Determine the Normal and Minimum Water Content.

Definitions
Normal Water Content: This is the water content of slurry yielding a consistency of 11 Bc.

Minimum Water Content:This is the water content of slurry yielding a consistency of 30 Bc.

69
17. THICKENING TIME TEST:
17.1. DEFINITION
This is the amount of time necessary for the cement slurry to reach a consistency of 100 Bc or poises,
at different well temperature, depth and pressure conditions. It also represents the length of time
the slurry is pumpable.

17.2. TEST PROCEDURE

1. After the cement slurry (Sample 1 Part (B)) is prepared, pour it immediately into the
Atmospheric Consistometer and begin stirring.
2. Record the consistency after every 4 minutes. Tabulate the results in the appropriate table.
3. Plot the Consistency in Bc versus time on a log-log paper and extrapolate the straight time to
100 Bc, to determine the thickening time.

70