DEPARTMENT OF PETROLEUM ENGINEERING

PETROLEUM ENGINEERING LABORATORY II REPORT

BY

AMAO TEMITOPE OLUSEGUN DEPARTMENT OF PETROLEUM ENGINNERING MATRIC NUMBER 145374

JULY, 2012.

AMAO TEMITOPE OLUSEGUN Department of Petroleum Engineering, Faculty of Technology, University of Ibadan, Ibadan. July 25th, 2012.

The Head, Petroleum Engineering Laboratory, University Of Ibadan, Ibadan. Dear Sir, SUBMISSION OF LABORATORY REPORT I, AMAO TEMITOPE OLUSEGUN with matriculation number 145374, write to bring to your notice that I have successfully completed the 2011/2012 session laboratory report. As required for a successful completion of TPE 416, I hereby tender this submission letter alongside my laboratory report, which contains comprehensive information as regards knowledge acquired during the laboratory experiments. I greatly appreciate your effort.

Yours faithfully,

Amao, Temitope Olusegun.

CONTENT

LABORATORY SAFETY---------------------------------------------------------------------------------------------------------- 3 EXPERIMENT 1 EXPERIMENT 2 EXPERIMENT 3 EXPERIMENT 4 EXPERIMENT 5 DETERMINATION OF SUURFACE TENSION-------------------------------------------------------- 5 DETERMIANTION OF DENSITY AND SPECIFIC GRAVITY---------------------------------------- 8 FLOW METER RIG EXPERIMENT-------------------------------------------------------------------- 12 MEASUREMENT OF LIQUID PERMEABILITY------------------------------------------------------ 17 MEASUREMENT OF GAS PERMEABIILITY--------------------------------------------------------- 21

REFRENCES----------------------------------------------------------------------------------------------------------------------- 24

LABORATORY SAFETY Safety in the laboratory requires the same kind of continuing attention and effort that is given to research and teaching. The use of new and/or different techniques, chemicals, and equipment requires careful preparation. Safety in the laboratory must be of vital concern to all those engaged in experimental science work. It is therefore the responsibility of everyone to adhere strictly to the basic safety precautions provided and to avoid any acts of carelessness that can endanger his life and that of others around him. There are five general principles of safety: 1. Practice safety. 2. Be concerned about the safety of others. 3. Understand the hazards associated with your particular experiment. 4. Know what to do in an emergency. 5. Report hazards or hazardous conditions.

1. Practice Safety Wear appropriate eye protection at all times. Use the hood for hazardous, volatile, and noxious chemicals. Smoking is prohibited in the building at all times. No food and drinks are allowed during the lab. Wear long pants and shoes with no open toes to avoid chemical exposures. Become familiar with your experiment before coming to the lab. Read the procedure thoroughly and study the equipment schematics before attempting to perform any experiment. 2. Be Concerned About the 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. This practice of looking out for the other person should include the practice of reminding a friend to wear safety glasses. Another aspect of this second principle involves alerting those around you of an accident and to alert personnel in the immediate vicinity of a fire or an emergency. Work as a team. Have someone in charge of the experiment whose job will be to coordinate what each one is doing. In case of confusion about any procedure, ask the instructor or the lab assistant. 3

3. Understand the Hazards Associated with Your Particular Experiment Prevention is the key to safety. It is important to know the potential hazards and safety precautions involved in a particular experiment. Hazards may include toxic substances, electrical circuits, mechanical equipment, and waste chemicals. Safety precautions should include correct material storage, proper ventilation, proper grounding of equipment, etc. It is equally important to always abide by all the instructions for conducting the experimental work during the laboratory sessions. Below are some guidelines for general laboratory safety and procedures: 1. All students must be familiar with the locations and operational procedures of the Emergency Shower, Fire Extinguishers, Gas Masks and Fire Blankets. 2. Laboratory coats, safety glasses and safety shoes MUST be worn at all times during the laboratory session. NO THOABS and open sandals are allowed during the laboratory sessions. 3. Eating, drinking and smoking are strictly PROHIBITED in the laboratory at all times. Laboratory glassware should NEVER be used for drinking purpose. 4. Report any injury immediately for First Aid treatment, no matter how small. 5. Report any damage to equipment or instrument and broken glassware to the laboratory instructor as soon as such damage occurs.

EXPERIMENT ONE TITLE: Determination of Surface Tension AIM: To determine the surface tension of a fluid sample. Apparatus: Tensiometer, spring, Beaker, Liquid sample. Special Note on the Use of the Ring Tensiometer The most common way of measuring the surface and interfacial tensions is with the ring method. The method is named after a French physicist who developed it in the late 1800's. In this method a platinum ring with defined geometry is immersed into the liquid and then carefully pulled out through the liquid surface. The measurement is performed by a Tensiometer, an instrument incorporating a precision micro balance, platinum-iridium ring with defined geometry and a precision mechanism to vertically move sample liquid in a glass beaker. The ring hanging from the balance hook is first immersed into the liquid and then carefully pulled up the surface of the liquid. The force applied on the ring while pulling through the surface is measured and plotted on a graph. The surface tension is the maximum force needed to detach the ring from the liquid surface. Special Note on Handling the Tensiometer 1. The platinum ring is very delicate and should be handled with utmost care. 2. Avoid touching the ring or the papers (used for calibration) with bare hand. Use tweezers for handling them. 3. When cleaning, clean the ring with the given test fluid and dry it while avoiding deformation of the ring. 4. Also do not touch the string which gives torsion to the lever arm. Procedure A. Preparatory Work 1. using a pair of holding instruments, place the platinum ring into the hook. 2. Set the zero of the Vernier scale and the main scale at the same mark. 3. Release the arrest mechanism. 4. Look onto the reference mark on the mirror and see if the pin hooked to the lever arm and the mark are at the same level. 5. If they are not at the same level, adjust the lever located at the far end of the string to adjust the torsion on the string and make the pin and the reference mark at the same level.

B. Measurement of Surface Tension 1. Arrest the lever arm and place the container with the test fluid on the platform and raise it by turning the platform adjusting knob. Stop when the ring is just immersed in the liquid. 2. Release the arrest mechanism and turn the knob to apply torsion on the string which eventually will raise the lever arm up. At the same time lower the platform so that the pin remains on the reference mark. Record the reading just at the ring breaks free from the liquid. 3. Take three or four readings. 4. Take the average of these readings, which will be used to calculate the surface tension. 5. Repeat the above steps for another sample.

Figure 1: Tensiometer OBSERVATION I observed that at the point when the ring was in contact with the surface of the distilled water, there was no movement or deflection of the Tensiometer. But the moment I rotated the knob on the 6

Tensiometer, there was a sudden separation that occurred between the clean ring and the surface of the distilled water and there was deflection of the reading on the Tensiometer. RESULT The surface tension recorded using distilled water as test sample was 43.5dynes/cm. THEORETICAL BACKGREOUND Surface tension is a phenomena observed at the surface of a liquid caused by the unbalanced forces acting on the molecular surface of the liquid in air. The surface or interfacial tension in the liquid film is the ratio of the surface force to the length (perpendicular to the force) along which the force acts.

=
Surface tension is basically used when characterizing gas-liquid interface. Surface tension is measured in dynes/cm. Surface tension decreases with an increase in pressure and temperature. PRECAUTIONS 1. I avoided error due to parallax when taking the Tensiometer reading by ensuring that I had a vertical view of the Tensiometer scale. 2. I ensured that the ring was dry before the experiment by using tissue paper to dry off the previous test sample from the ring. CONCLUSION The surface tension is an important property in reservoir engineering calculations and designing enhanced oil recovery projects.

EXPERIMENT TWO Title: Determination of density and specific gravity Aim: to determine the density and specific gravity of fluid samples at different temperatures. Apparatus: Pycnometer (density bottle), water bath, thermometer, acetone, water, crude oil, beakers, electric weighing balance. Procedure (for crude oil as test sample) 1. I rinsed the Pycnometer bottle with acetone which is a volatile substance so as to ensure that the density bottle is dry. 2. I weighed the Pycnometer when it was dry and empty so as to determine its weight. 3. I filled the Pycnometer (density bottle) with the given crude oil sample and inserted the stopper thereby making sure that the hole in the stopper is filled. 4. I hung the density bottle (Pycnometer) in the water bath at the given temperature and allowed 5 minutes to attain equilibrium. 5. I removed the Pycnometer from the water bath and wiped dry. 6. I weighed the Pycnometer plus sample on the weighing balance and took the reading. 7. I repeated the procedure at different temperatures. The result is presented in the table below.

Pycnometer Figure 2

Water bath

Result T/oC 44.5 56.5 67.0 77.0 84.5 T=Temperature (oC) Wp=Weight of dry Pycnometer (g) Wop= Weight of Pycnometer filled with oil (g) Wo= Weight of oil (g) Vo= Volume of density bottle (Pycnometer) (cm3) = 50ml= 50cc Procedure for water as test sample 1. I rinsed the Pycnometer bottle with acetone which is a volatile compound so as to ensure that the density bottle is dry. 2. I weighed the empty and dry Pycnometer to determine its weight. 3. I filled the Pycnometer with water and inserted the stopper thereby making sure that the hole in the stopper is filled. 4. I hung the density bottle in the water bath at the given temperature and allowed 5 minutes for equilibrium. 5. I removed the Pycnometer from the water bath and wiped dry, I thereafter weighed it. RESULT T/oC 38.0 49.0 59.5 66.0 77.0 T=Temperature (oC) Wp=Weight of dry Pycnometer (g) Wwp= Weight of Pycnometer filled with water (g) Wp/g 20.49 20.49 20.49 20.49 20.49 Wwp/g 71.2 71.0 70.8 70.6 70.5 Ww/g 50.71 50.51 50.31 50.11 50.01 Vo/cc 50.0 50.0 50.0 50.0 50.0 w/(g/cc) 1.0142 1.0102 1.0062 1.0022 1.0002 Wp/g 19.91 19.91 19.91 19.91 19.91 Wop/g 66.33 66.10 65.63 65.63 65.06 Vo/cc 50.0 50.0 50.0 50.0 50.0 o/(g/cc) 0.9284 0.9238 0.9144 0.9108 0.9030

Ww= Weight of water (g) Vw= Volume of density bottle (Pycnometer) (cm3) containing water = 50ml= 50cc Table of Specific gravity and API gravity T/oC 44.5 56.5 67.0 77.0 84.5 Wp/g 19.91 19.91 19.91 19.91 19.91 Wop/g 66.33 66.10 65.63 65.45 66.06 Wo/g 46.42 46.19 45.72 45.54 45.15 o (g/cc) 0.9284 0.9238 0.9144 0.9108 0.9030 w/(g/cc) 1.0062 1.0062 1.0062 1.0062 1.0062 SG 0.9227 0.9181 0.9088 0.9051 0.8974 API 21.85 22.62 24.20 24.84 26.18

SG= Specific Gravity= API Gravity= APIo= OBSERVATION

1. I observed that the crude oil flowed out of the density bottle stopper as the density bottle was heated in the water bath. 2. From the result, I observed that there was a decrease in density and specific gravity as temperature increased. 3. I observed that the variation of density of the water with respect to temperature was minute (very small). THEORETICAL BACKGROUND Density () is defined as the mass of the fluid per unit volume. In general, it varies with pressure and temperature. The dimension of density is kg/m3 in SI or lb/ft3 in the English system. Specific gravity () is defined as the ratio of the weight of a volume of liquid to the weight of an equal volume of water at the same temperature. The specific gravity of liquid in the oil industry is often measured by some form of hydrometer that has its special scale. The American Petroleum Institute (API) has adopted a hydrometer for oil lighter than water for which the scale, referred to as the API scale, is API Gravity= APIo= When reporting the density the units of mass and volume used at the measured temperature must be explicitly stated, e.g. grams per millilitre (cm3) at T (OC). The standard reference temperature for international trade in petroleum and its products is 15 OC (60 OF), but other reference temperatures may be used for other special purposes.

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The Pycnometer is an accurately made flask, which can be filled with a known volume of liquid. The specific gravity of liquid is defined as the ratio of the weight of a volume of the liquid to the weight of an equal volume of water at the same temperature. Both weights should be corrected for buoyancy (due to air) if a high degree of accuracy is required. The ratio of the differences between the weights of the flask filled with liquid and empty weight, to the weight of the flask filled with distilled water and empty weight, is the specific gravity of the unknown fluid. The water and the liquid must both be at the same temperature. PRECAUTION 1. 2. 3. 4. When the stopper was inserted, I ensured that it was filled with the sample fluid. I ensured that the Pycnometer did not come in contact with the base of the water bath. I ensured that the thermometer did not ouch the base of the water bath. I avoided error due to parallax when taking the reading from the thermometer.

CONCLUSION The experiment is useful in obtaining the densities and specific gravities of the crude oil at different temperatures since the density and specific gravity are temperature dependent.

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EXPERIMENT THREE Title: Flow Experiment Aim: To determine the head losses of different flow measuring devices. Objective: To compare and contrast the head losses in the orifice plate (orifice meter) and venture meter when a liquid flows through them. Apparatus: The flow rig consisting of: a centrifugal pump that circulates water through the system, a water reservoir for water storage, a manometer which measures the differential pressure between the entry and exit of each measuring device, a water level indicator which indicates the volume of water that has accumulated in a drainable volumetric tank, flow measuring devices (orifice plate and venture tube). Other apparatus are stop watch and the water used as the flowing liquid. Procedure for the orifice plate 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. I filled the tank with the water to the brim. I connected the rubber hose from the orifice to the big manometer appropriately. I regulated the water level in the arms (P1 and P2) of the big manometer to equal level. I regulated the water level in the two arms (P1 and P2) of the big manometer to equal level. I turned the water pump valve to zero point. I connected the equipment to power supply and switched the flow-rig power on. I started the stop watch when the water level in the small manometer is stabilized. I stopped the watch when the water has moved from 0.5 as indicated on the small manometer. I took the reading off the big manometer and recorded the time taken. I subtracted P2 from P1 Subsequent readings were obtained by increasing the flow rate from the pump and following the procedure outlined above.

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Figure 3: Flow Rig THEORETICAL BACKGROUND This experiment was aimed at measuring the head loss between the inlet and the outlet points of a measuring device. This is done by determining the coefficient of discharge of the flow through each device. The principle is based on the theory that energy is lost when a flowing fluid velocity is reduced by constricting its path of flow. The energy losses are measured in terms of the head loss experienced by the fluid. In a flow metering device based on the Bernoullis equation, the downstream pressure after an obstruction will be lower than the upstream pressure before. To understand orifice, nozzle, and venture meters, it is necessary to therefore explore the Bernoullis equation. Assuming a horizontal flow (neglecting minor elevation differences between measuring points), the Bernoullis equation can be modified to:

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v2 2 v12 p1V1 p2V2 2 g 2 g (1)

Where P= pressure v= flow velocity V= specific volume The equation can be adapted to vertical flow by adding elevation heights h and h. Assuming uniform velocity profiles in the upstream and downstream flow, the continuity equation can be expressed as q= VA= VA..(2) Where q= flow rate A= flow area Eq. 1 may be simplified by assuming that V = V = V, an assumption that is approximately true and is later corrected by a term called the expansion factor. Then, v - v = 2gV (p - p) = 2gh The term h is the differential head loss between points 1 and 2 expressed as feet of fluid (the fluid flowing in the system). The velocities may be expressed in terms of volume flow rate g and diameters d and d (internal diameter of pipe and orifice opening respectively). This substitution yields an intermediate equation. Combining equations (1) and (2) gives

A2 2 gh 1 4
.. (3)

Where

A2

= area of orifice plate opening

d = orifice, venture, or nozzle inside diameter d = upstream and downstream pipe diameter 14

 = d/d diameter ratio

The theoretical flow rate q will in practice be smaller (2-40%) due to geometrical conditions. The ideal equation (3) can be modified with a discharge co-efficient,

Cd

q Cd

A2 2 gh 1 4

Figure 4: Flow through Orifice Plate ORIFCE PLATE Volume(cc) 5000 5000 5000 5000 5000 5000 5000 P1(mmH2O) 460 440 428 685 415 434 418 P2(mmH2O) 430 320 322 320 327 330 330
P1-P2(mmH2O)

Time (s) 244.0 173.0 170.0 62.0 148.0 144.0 146.0

Q= (cc/s) 20.49 28.90 29.41 80.65 33.78 34.72 34.25

H= 3.06 12.23 10.81 37.21 8.97 10.60 8.97

30 120 106 365 88 104 88

H=

=Density of water=(g/cc) g=acceleration due to gravity

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OBSERVATION 1. I observed that the higher the pressure difference between the inlet and the outlet of the orifice plate, the lower the time required for the 5000cc to flow and subsequently, the lower the flow rate. PRECAUTIONS 1. The level of water in the reservoir was checked at intervals to ascertain it was above the critical level. 2. I ensured that the two manometer readings were at the same level before flow began. 3. I ensured that the stop watch was started at the instant flow began and stooped it when flow ended.

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EXPERIMENT FOUR Title: Measurement of Liquid Permeability Aim: To determine the liquid permeability of a core sample. Apparatus: Core holder, Calibrated cylinder, stop watch, flow pump.

Figure 5: Core holder and Liquid Permeameter PROCEDURE 1. I loaded the 100% saturated core plug into the core holder and applied appropriate overburden pressure of 0.25psi. 2. I flowed several volumes of distilled water through the sample so a s to ensure a steady laminar flow. 3. I started the stop watch and measured 5cm3(5ml) of liquid water into a calibrated test tube at the point of first drop. 4. When the 5ml calibrated cylinder was full, I stopped the stop watch and noted the reading.

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Figure 6: Liquid Permeameter THEORETICAL BACKGROUND Permeability is a measure of the ease with which a formation permits a fluid to flow through it. Permeability is a property of the porous medium and is a measure of the capacity of the medium to transmit fluids. Permeability is an INTENSIVE property of a porous medium (e.g. reservoir rock). To be permeable, a formation must have interconnected porosity (intergranular or intercrystalline porosity, interconnected vugs, or fractures). Permeability is measured in Darcy units or more commonly millidarcy (md - one thousandth of a Darcy) after Henry Darcy who carried out some pioneering work on water flow through unconsolidated sandstones. It is defined by the equation which expresses Darcy's law. Generally stated as: K= Q= the total discharge of fluid per unit time (cm3/s) A= the cross-sectional area of the flow path (cm2) L= the length of the flow path (cm)

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= Dynamic fluid Viscosity (centi poise) K= the permeability in Darcy P1 P2 = Pressure difference (atm) To determine the permeability of a formation, several factors must be known: the size and shape of the formation, its fluid properties, and the pressure exerted on the fluids, and the amount of fluid flow. The more pressure exerted on a fluid, the higher the flow rate. The more viscous the fluid, the more difficult it is to push through the rock. Viscosity refers to a fluids internal resistance to flow, or its internal friction. For example, it is much more difficult to push honey through a rock than it is to push air through it. Permeability is measured in Darcy. Few rocks have a permeability of 1 Darcy, therefore permeability is usually expressed in millidarcies or 1/1000 of a Darcy.

RESULT Length (L) of core sample= 5.71cm Diameter= 3.785cm Radius= Area of cross section= r2= 3.142 x 1.89252= 11.246cm2 Viscosity= 0.89cp The observed time (T) = 1.8 minutes K= = Differential Pressure= 0.25psi K= K= k=1209.5mD Flow rate= PRECAUTIONS 1. I avoided error due to parallax when reading the time from the stop watch. 2. I ensured the stop watch was stopped the instant 5ml liquid volume was filled. 19 = = 0.0463cc/s

3. I pre saturated the core for 24 hours. CONCLUSION The calculated permeability of 1209.5mD indicates that the sample has an excellent permeability. This is consequent upon the fact that there is a high degree of interconnectivity between the pore spaces.

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EXPERIMENT FIVE Title: Measurement of Gas permeability in a porous medium Aim: To determine the permeability of a porous media using nitrogen gas. Apparatus: core holder, end stem, rubber boot, core plug, stop watch, bubble tube flow meter, pressure gauge.

Figure 7: Gas Permeameter THEORETICAL BACKGROUND Permeability is a property of the porous medium that measures the capacity and ability of the formation to transmit fluids. The rock permeability, k, is a very important rock property because it controls the directional movement and the flow rate of the reservoir fluids in the formation. This rock characterization was first defined mathematically by Henry Darcy in 1856. In fact, the equation that defines permeability in terms of measurable quantities is called Darcys Law. Darcy developed a fluid flow equation that has since become one of the standard mathematical tools of the petroleum engineer. If a horizontal linear flow of an incompressible fluid is established through a core sample of length L and a cross-section of area A, then the governing fluid flow equation is defined as;

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V=Where v = apparent fluid flowing velocity, cm/sec k = proportionality constant, or permeability, Darcys = viscosity of the flowing fluid, cp dP/dL = pressure drop per unit length, atm/cm Standard laboratory analysis procedures will generally provide reliable data on permeability of core samples. If the rock is not homogeneous, the whole core analysis technique will probably yield more accurate results than the analysis of core plugs (small pieces cut from the core). Procedures that have been used for improving the accuracy of the permeability determination include cutting the core with an oil-base mud, employing a pressure-core barrel, and conducting the permeability tests with reservoir oil. Permeability is reduced by overburden pressure, and this factor should be considered in estimating permeability of the reservoir rock in deep wells because permeability is an isotropic property of porous rock in some defined regions of the system, that is, it is directional. Routine core analysis is generally concerned with plug samples drilled parallel to bedding planes and, hence, parallel to direction of flow in the reservoir. PROCEDURE 1. I determined the length, diameter and cross sectional area of the plug sample. 2. I inserted the plug into the rubber boot and attached to end stems to either side. 3. I loaded everything into the core holder and screwed down the core holder (from the gas regulator). I connected the down stem line from the core holder to the Permeameter. 4. I opened the gas cylinder using the gas regulator and injected gas into the sample and watched as the gas lifted a single bubble in the bubble tube (burette). 5. I adjusted the pressure regulator to ensure laminar flow. 6. Using the stop watch, I timed the bubble time of travel over 25cc to determine the flow rate. 7. I disconnected the entire setup and calculated permeability using Darcys law. RESULT Length L= 5.731cm Diameter D= 3.785cm Radius= Area of cross section= r2= 3.142 x 1.89252= 11.246cm2 Viscosity = 0.177cp

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Observed time= 50.50 Seconds P1= 1.5psi P2=0 psi Flow rate= = = 0.495cc/s

Flow rate= Q= 0.495cc/s K= K= K= 0.0298 Darcy K= 29.18mD PRECAUTIONS 1. I ensured that the flow rate was less that 1cc/second all through the experiment for Darcys law to hold. 2. The rubber tube joining the permeameter to the pressure cylinder was properly fitted to prevent gas leakage. CONCLUSION The calculated permeability for gas (29.78mD) indicates that the core sample is fairly permeable. As a result, it can be inferred that the interconnectivity between the pore spaces is low. The permeability is low as a result of the tightness and consolidation of the sample used.

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REFRENCES 1. Amyx J.W., Bass Jr. D.M. and Whiting R.L.: Petroleum Reservoir Engineering, McGraw-Hill, 1960. 2. Bear J.C.: Dynamic of Fluids in Porous Media, American Elsevier, 1972. 3. Koederitz L.F., Harvey A.H. and Honarpour M.: Introduction to Petroleum Reservoir Analysis; Laboratory Workbook, Gulf Pub. Co., 1989. 4. EZ Tensiometer (Model 101) Instruction Manual, Temco Inc, Tulsa, OK, USA.

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