LABORATORY MANUAL FOR DRILLING FLUIDS AND CEMENTS AND RIG FLOOR SIMULATION

PNG 451 OIL WELL DRILLING LABORATORY

Petroleum and Natural Gas Engineering The Pennsylvania State University 9th Edition, 2010

Copyrighted @ 2010 PSU

FIELD TESTING OF DRILLING FLUIDS

INTRODUCTION Every drill operation depends directly upon the properties of the drilling fluid. The properties of the drilling fluid should be such as to promote safe and speedy drilling and completion of the well with the maximum productive capacity. The use of drilling muds of controlled properties frequently requires considerable sums of money. These expenditures must be justified and it is well to examine the role of the drilling fluid to determine its necessary properties. The general functions of a drilling fluid are: 1. Cooling and lubricates the bit and drill pipe. 2. Removing cuttings from the hole. 3. Preventing settling of cuttings in the hole when circulation stops and allowing dropping of cuttings in the surface circulating system. 4. Depositing an impermeable wall cake. 5. Overcoming formation pressures to prevent influx of oil, gas, or water. 6. Preventing caving of the formation. 7. Preventing contamination of the producing formation. 8. Allowing good electric logs to be taken. 9. Reducing casting and cementing costs. 10. Preventing drill pipe corrosion. Of all the mud systems in use today, the fresh water type is the basic, most universally used mud system. The remaining mud systems have been developed to overcome drilling conditions which fresh water muds have difficulty in handling or for which they are totally unfitted. However, as we shall see, it is probably impossible for any one mud system to satisfy all the necessary functions of a drilling fluid. Consequently, the choice of mud type for a specific instance is governed by those functions which are the most critical to the well in question, and some sacrifice of other desirable properties must be made. Prepared as a guide, this section first discusses field tests that evaluate drilling fluids, especially muds, by measuring certain properties of the drilling fluid and its filtrate. To associate these tests more closely with drilling conditions, the significance of each test as a factor of proper mud control, and, in turn, the importance of mud control to successful drilling, are pointed out briefly. Second, this section details a series of experiments to help the student better understand drilling muds.

TEST PROCEDURES
DENSITY (Mud Weight) It is extremely important that the density of the drilling mud be known throughout the drilling operation. This is true whether drilling through gas, oil, or saltwater sands; shale, where relatively high density may be required; or into low pressure production zones, where low density colloidal mud is advantageous. Frequent density tests aid in preserving a safety factor by disclosing any changes taking place in the unit weight of the mud. The most practical instrument for measuring mud density is the Mud Balance. Mud Balance The Mud Balance provides a simple method for the accurate determination of mud density. Durably constructed, it consists principally of a base and graduated arm with cup, lid, knife edge, rider, level, and counterweight. Procedure: 1. Remove lid and fill cup to the top with sample to be tested. (When testing mud, first remove air and other gases from sample using the Baroid Mud Dearator.) 2. Replace lid and rotate until firmly seated, making sure some sample squeezes out the vent hole. 3. Wipe sample from exterior of balance. 4. Place balance on base with knife edges on fulcrum rest. 5. Move rider until instrument is in balance, as determined by level. 6. Read sample density at end of rider nearest fulcrum. Results: The instrument must first be calibrated by using distilled water as the sample. After measuring the density of the water, dry the cup and then measure the density of the mud. Calculate the true mud density (corrected for balance error) using the following formula:

Measured density of distilled water Measured mud density = True density of distilled water True mud density The density of distilled water is 8.33 pounds/gallon or 62.4 pounds/cubic foot. (Alternately, balance error of the Mud Balance can be eliminated by adding or removing lead shot from the counterweight.) In most parts of the world mud weight is expressed in pounds per gallon (ppg). In California,
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many companies use pounds per cubic foot.

VISCOSITY

Viscosity is a measure of the internal resistance of a fluid to flow: the greater the resistance, the higher the viscosity. For drilling operations, viscosity of mud must be controlled and a standard means of measuring viscosity provided. Hole size, hole condition, pumping rate, drilling rate, cutting size, cavings, presence or absence of shale separators, mud weight, design of the pit systems, and gel characteristics of the mud are factors influencing the specification of the viscosity of any given mud. The development of satisfactory instruments for measuring the viscosity of drilling muds has been the subject of much effort. This is due largely to the fact that drilling fluids are fundamentally thixotropic and the viscosity characteristics of such materials cannot be described by means of a single measurement. The indicated viscosity as obtained on any instrument is valid only for that rate of shear and will differ when measured at a different rate of shear. Two instruments for determining will be described: the Marsh Funnel Viscosimeter and the Baroid Rheometer (which is similar in operation to a Fann V-G Meter.)
Marsh Funnel Viscosimeter

The Marsh Funnel Viscosimeter is used for routine viscosity determinations on nearly every drilling rig. The measurement obtained is influenced considerably by rate of gelation and by density which varies the hydrostatic head of the column of mud in the funnel. Because of these 4

variations, the viscosities obtained with the Marsh Funnel cannot be correlated directly with those found using rotational viscosimeters. Marsh Funnel viscosities are of little quantitative use but have general comparative value.
Procedure:

1. Hold funnel in upright position with index finger over outlet. (Instead of holding funnel, it may be placed in a ring stand.) 2. Pour the test sample freshly taken from the mud system, through the screen in top of funnel until mud level just reaches the underside of the screen. (The funnel now contains 1500 cc of mud.) 3. Immediately remove finger from outlet tube and measure number of seconds for one quart (946 cc) of the sample to run out. This time in seconds is recorded as the Marsh Funnel Viscosity of the mud. Also report the temperature of the sample.

Baroid Rheometer

The Baroid Rheometer is a rotational viscosimeter with which one, two, or multiple point viscosities. Its fixed speeds of 3 (GEL), 100, 200, 300, and 600 RPM are switch selectable with the RPM knob. In addition, the same switch, when set to the VAR position, enables the operator to select any speed between 3 and 625 RPM by annually adjusting the VARIABLE knob.
Procedure:

1. Place a recently agitated sample in the mud cup, and tilt the instrument head into the field. Adjust the head with the knurled knob until the rotor sleeve is immersed to the scribed line. 2. Stir the sample for about 15 seconds at 600 RPM.

3. Read the meter deflection at the following RPMs: 3 (GEL), 10, 25, 50, 75, 100, 200, 300, and 600. (NOTE: The meter whose deflection is to be read is labeled VISCOSITY. This label is incorrect. The meter deflection indicates shear stress; to calculate viscosity, see below.)
Results:

1. The plastic viscosity (PV), in cp, is calculated by: Plastic Viscosity = 600 300 = P 2. The apparent viscosity at each RPM, in cp, is calculated by: Apparent Viscosity =

300 300 = A RPM

3. The Bingham yield point (YP), in pounds/100 square feet, is calculated by: Bingham Yield Point = 300 P 4. Plot vs. RPM, as shown in Gatlin.

SHEAR OR GEL STRENGTH

The gel strength of drilling muds is a measure of the minimum shearing stress necessary to produce slip wise movement. Two readings are generally taken: the first, immediately after agitation of the mud in the cup; the second, after the mud in the cup has been quiescent for a period of ten minutes. The readings are referred to as the initial gel strength and the ten - minute gel strength, respectively. Both gel strength readings so determined will be zero for nonthixotropic fluids, such as water and brines, no matter how viscous but the difference in the readings may be appreciable for suspensions such as drilling muds. The difference is considered to be a measurement of the thixotropic of the mud system. Hole size, type of formations, depth, temperature and pressure of formation fluids or gases, and amount of weight material in the mud are factors that must be considered in prescribing desirable gel-strength properties of the mud. The Marsh Funnel has been used to some degree to obtain a measure of the gel strength of muds. In making the gel strength test the viscosity time in seconds is first determined with minimum delay between filling the funnel and making the measurement as described previously. The funnel is then refilled and allowed to stand quiet for ten minutes, after which the viscosity is again measured. The time difference in seconds between the first and second measurements gives the gel strength in seconds. This method is not recommended and is given largely for historical reference. The Baroid Rheometer is commonly used to measure gel strength.
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Baroid Rheometer Procedure:

1. Stir a sample at 600 RPM for about 15 seconds. 2. Turn the RPM knob to STOP; allow the desired rest time (10 seconds for ten second Gel strength; 10 minutes for ten minutes Gel strength) and then turn. 3. Switch the RPM knob to the GEL position; the maximum deflection of the dial before the gel breaks is the Gel strength in pounds/100 square feet.

FILTRATION PROPERTIES

The filtration properties of drilling muds are a measure of the ability of the solid components of the muds to form a thin, low-permeability filter cake. The lower the permeability, the thinner the filter cake and the lower the volume of filtrate from muds of comparable solids concentration. This property is dependent upon the amount and physical state of the colloidal material in the mud. It has been shown repeatedly in the field that when mud of sufficient colloidal content is used, drilling difficulties are minimized. In contrast, a mud low in colloids and high in inert solids deposits a thick filter cake on the walls of the hole. A thick filter cake restricts the passage of tools and allows an excessive amount of filtrate to pass into the formation, thus providing a potential cause of caving and differential pressure wall sticking. Lack of proper walling properties may result in further trouble such as difficulty in running casing, creating a swabbing effect which may cause the formation to cave or swab reservoir contents into the hole, and difficulty in securing a water shutoff because of channeling of 7

cement. The filtration properties will be studied with two pieces of equipment: The Filter press and the Mud Sticking Tester.
Filter Press

The filtration, water loss, or wall building test is conduced with a Filter press. The test consists of measuring the rate at which filtrate (the continuous liquid phase of the mud) is forced from the sample under a specified pressure of 100 psig. Both the filtrate volume (ml) and the mud cake thickness (32nd of an inch) are reported. The Filter Press consists of a mud reservoir mounted on a frame, a filtering medium, a means of catching and measuring the filtrate, and provisions for a pressure source. The filtering medium is a sheet of especially hardened filter paper which fits on a screen in the base cap.
Procedure:

1. Assemble the following dry pans in this order: base cap, screen, a sheet of filter paper, rubber gasket, and cell. Secure the cell to the base cap. 2. Fill the cell with the sample to be tested to within of the top. Set the unit in place in the filter press frame. Check the top cap to make sure the gasket is in place. Place the top cap on the cell and secure the unit in place with the T-screw. 3. Place a dry graduated cylinder under the filtrate tube. 4. With the regulator T-screw in its maximum outward position (closed position), open the valve to the cell. Apply a pressure of 100-psig to the filter cell by rapidly screwing the regulator T-screw into the regulator. Timing of the test should begin now. 5. Record the initial filtrate loss; then record the filtrate loss every minute for the first 7.5 minutes (also record the loss at 7.5 minutes); then record the loss at 10, 15, 20, 25, and 30 minutes (end of test). 6. Close the valve to the cell rapidly and open the safety-bleeder valve. Return the regulator T-screw to its maximum outward position.
Results:

1. Plot filtrate volume vs. square root of time (as shown in Gatlin, p.74). Determine the collected 30 minutes filter loss. 2. The filter cake thickness is determined after the cell has been disassembled. The filter paper with the cake deposited on it is removed from the base cap, and excess mud is gently washed from the cake with a gentle stream of water. The filter cake thickness is measured and reported in thirty-seconds of an inch. 3. Properties of the filter cake such as texture, hardness, flexibility, etc., may be reported.

Mud Sticking Tester

The sticking tendency of a mud filter cake is measured with the Baroid Mud Sticking Tester. The torque required to free a steel disk in contact with a mud filter cake is measured and used in the calculation of the sticking coefficient. The sticking coefficient is an indication of the force required to rotate (or free) a section of drill pipe in contact with the wall cake in the borehole. The sticking coefficient can be used to evaluate the cake lubricity of various muds.

Procedure:

1. Start with a clean apparatus. Be especially sure that the torque plate is clean, Scour the face of the plate with abrasive cleanser until the plate shines and rinse thoroughly with water. Then dry carefully. 2. Place filter paper, rubber gasket, the slip ring on screen inside chamber. Screw hold-down ring over gaskets, using ring wrench. 3. Insert threaded end of one of the valve stems into bottom center hole of cell and turn hand tight. 4. Fill cell with mud sample to the scribed line. 5. Set cell on stand mating the four tips into stand holes. 6. Slip torque plate stem through lid with polished surface facing up looking at inside of lid. 7. Put lid onto cell with stem of torque plate standing up through O ringed center hole of 9

lid. Tighten cell lid with Spanner Wrench, using torque plate level for a backup. 8. Insert the other valve stem in cell lid and tighten hand tight (closing valve). 9. Set CO2 assembly over top end of valve stem and insert locking pin. 10. Turn relief valve on CO2 assembly to closed position. Back out regulator handle. 11. Insert CO2 cartridge into knurled CO2 holder, and tighten holder onto head puncturing cartridge. 12. Place graduate under cell and turn lower valve stem a quarter turn back from hand tight, thus opening the valve. 13. Turn regulator handle in until 500 psi is read gage. 14. Pull plate stem up and hold there while opening top valve stem by turning stem a quarter turn back from hand tight. 15. Record the time for the start of test. 16. Allow the mud to filter to desired cake thickness or filtrate volume, then push torque plate down using the torque plate lever. To do this, catch the groove in the bar in the column top cross support and hold plate down until pressures equalize allowing plate to stick. 17. Record filtrate volume and time. 18. Allow plate to stick for 5 minutes or more. Put socket on torque wrench. Zero dial on torque wrench. Place the torque wrench and socket on the hex top of the torque plate stem, and measure the torque wrench while watching dial. With free hand, for a backup, use the torque plate level wedged between columns above cell platform. 19. Record set time (i.e. plate sticking time), filtrate volume, and maximum torque. 20. Repeat steps 18 and 19 for additional readings. 21. Back off regulator handle and then open bleed-off valve. 22. Pull pin, remove CO2 assembly and remove top valve stem. Loosen cell lid with Spanner Wrench, unscrew lid, and pour mud out of cell. 23. Disassemble apparatus and wash thoroughly, being careful not to scratch the torque plate.

Results:

1. The sticking coefficient is the ratio of the force necessary to initiate sliding of the plate to the normal force on the plate, and is given by:

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Sticking Coefficient = where:

1.5 T A P

T = maximum torque, in inch-pounds. A = plate area, in square inches. P = differential pressure, in psi

For this instrument, A = 3.14 in2 and P = 500 psi (as specified in step 13). 2.Plot sticking coefficient versus set time.

HYDROGEN ION CONCENTRATION

The degree of acidity or alkalinity of drilling mud is indicated by the hydrogen ion concentration that is commonly expressed in terms of pH. The hydrogen ion concentration of a drilling mud exerts considerable influence on its properties and hence is of interest to the petroleum engineer. pH control is also important in corrosion control, usually pH is kept above 10 for this reason. Water dissociates slightly into hydrogen ions and hydroxyl ions. It can be shown that at a given temperature the product of the concentrations of these ions is a constant. That is: (H+) (OH-) = K = l x 10-14 (at 25 C) In pure water the concentrations of these two ions are equal and each is 10-7 moles per liter. The addition of an acid will increase the concentration of hydrogen ions with a corresponding decrease in hydroxyl ion concentration. Thus, if a water solution contains one mole per liter of hydrogen ions, then the hydroxyl ion concentration must be 10-14 moles per liter by the above expression for the dissociation of water. Conversely if the solution is made basic there will be a corresponding decrease in hydrogen ion concentration. The product of the two ion concentrations will, however, remain constant. The pH of a solution is a measure of its hydrogen ion concentration. pH is defined as:
1 pH = log + H + = log H

( )

Thus in pure water ( H+) = (OH-) = 10-7 and the pH is 7. A solution containing one mole of hydrogen ion per liter would have (H+) = l and the pH is 0. The pH measurement is used as an aid in determining the need for chemical control of the mud as well as indicating the presence of contaminants such as cement, gypsum, etc. The opening pH for any drilling muds is commonly measured with an electronic pH Meter.

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pH Meter

The electromatic hydrogen ion determination offers a fast, accurate determination of pH. The operation of these meters involves the generation of an electric potential in a glass and calomel electrode system by the solution under test. The electrical potential is amplified by means of a vacuum-tube system and the reading is indicated directly on a meter.
Procedure:

1. Check battery by turning selector to BAT CK. 2. Turn selector to STANDBY position. Selector must be kept in this position while rinsing, removing, or inserting electrodes to prevent damage to delicate electronic components. 3. Remove plastic end cap and soak electrode in distilled water a few minutes, then wipe with soft tissue. 4. Add sufficient buffer solution to a test tube to cover the electrode when inserted (use buffer of pH in range expected of mud pH). Insert electrode. 5. Set temperature knob to the solution temperature. 6. Turn selector to READ, IMPORTANT, Do not electrode in your hand while taking reading. Remove hand at least 12 inches away. Local radio transmission and electric fields often conduct through the human body and cause shifts in readings. 7. Set meter to pH of buffer with STANDARIZE knob. 8. Turn selector to STANDBY. Note: By noting reading in this position, electronics drift can be compensated by bringing the meter back to this reading with STANDARDIZE knob, thus avoiding frequent buffering. 9. Remove electrode and rinse with distilled water. 10. Insert electrode into solution to be tested. 11. Turn selector to READ. 12. Stir carefully to assure fresh solution. Wait adequate time for a steady reading. Make sure temperature knob is set correctly. Remove hand from electrode before reading. 13. Turn selector to STANDBY = = before removing electrode from solution. 14. To run next sample, repeat steps 9 through 11. 15. When finished, turn selector to OFF. Rinse electrode in distilled water and wipe clean with soft tissue. 16. Before storing, wet electrode with a few drops of pH 7 buffer and replace plastic protector.

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RESISTIVITY

Control of the resistivity of a mud and mud filtrate while drilling may be desirable to permit better evaluation of formation characteristics from electric logs. A salt mud (low resistivity) will prevent the obtaining of a good, definitive SP curve. The determination of resistivity is essentially the measurement of resistance to flow of electrical current through a known configuration of a sample. Measured resistance is converted to resistivity by use of a cell constant. The cell constant is fixed by the configuration of the sample in the cell and is determined by calibration with standard solutions of known resistivity. The resistivity is expressed in ohm-meters. Any type of cell and instrument which is sufficiently accurate to permit determination of resistivity within five percent of the correct value may be used. If the instrument indicates the sample resistance in ohms, the cell constant must be known. The resistivity in ohm-meters is obtained by multiplying the resistance in ohms by the cell constant in square meters per meter. If the instrument is a type of direct-reading resistivity meter, the cell constant has been adjusted to a particular value or accounted for in the circuitry of the meter. Such an instrument measures the sample resistance and converts it to the resistivity so that the reading is taken directly in ohmmeters.
Baroid Resistivity Meter

The Baroid Resistivity Meter is a transistorized electrical meter for measuring the resistivity of fluids, slurries, or semi-solids having resistivities of 0.01 to 10 ohmmeters. (The instrument reads directly in ohm-meters.) Conductivity of the medium being measured is obtained by taking the reciprocal of the resistivity measurement.

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Procedure: Filtrate and Mud

1. Fill cell with fluid, being careful to remove all air bubbles (fill and exhaust fluid two or three times to thoroughly wet the surface). 2. Connect cell to the meter. 3. Press the black button and adjust for full scale reading on the meter. 4. While keeping the black button depressed, press the red button. 5. The reading on the meter is the resistivity of the fluid. (When testing mud, it may be necessary to allow 3 to 5 minutes after putting mud in the cell before taking a reading to allot the cell and mud to reach temperature equilibrium.) 6. Record the resistivity reading and the cell temperature. 7. Remove the cell and clean with distilled water. (Pipe cleaners can be used to remove mud that cannot be flushed out with water.)
Procedure: Mud Cake

1. Remove excess water from filter cake. 2. Fill the slot on top of the cell with mud cake. 3. Press black button and adjust for full scale. 4. While keeping the black button depressed, press red button. 5. The reading on the meter is the resistivity of the mud cake. 6. Record the resistivity of the mud cake and the cell temperature. 7. Remove the cell and clean thoroughly with distilled water.

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Note:

1. Use only fresh or distilled water (mild soaps only when necessary) to clean the cell. Do not use any type of solvent. Do not scratch the inner surface of the cell when using a pipe cleaner. 2. When full-scale reading cannot be obtained when the black button is depressed, the battery needs to be replaced. Use a 22.5 V Burgess U-15 or equivalent. Be sure to observe polarity when replacing the battery in order to prevent damage to the transistor.

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FIELD TESTING OF OIL WELL CEMENTS

INTRODUCTION

The discovery of Portland cement dates back to 1824 when Joseph Aspdin, an English mason, was issued a patent covering gray, rock-like material called cement. This cement was produced by feeding a finely ground mixture of limestone, clay, into a rotating kiln at 2600 F. As this mixture traveled through the kiln it was convened into cement clinker. The clinker was then stored in bins and later ground with gypsum (retarded setting time and added strength) to form the final cement. It was not until the early 1900s, through, that the use of cement in oil well operations was introduced. In 1903, Frank F. Hill used a cement slurry to shut off down-hole water just above an oil sand in the Lompoc field in California. Since that time no other production operation has played as important a role in the producing life of an oil well. Basically, oil-well cementing is a process of mixing a cement-water slurry and pumping down steel casing to critical points located in the annulus around the casing, in the open hole below or in fractured formations. This operation is referred to as primary cementing. Its main functions are to (1) support the casing, (2) seal off non-productive formations, and (3) retard corrosion by minimizing casing contact with saline formation waters. Secondary cementing deals with completion and remedial repairs on a well after the producing zone is reached. Squeeze-cementing, the most common form of secondary cementing, involves applying hydraulic pressure to force or squeeze a cement slurry in contact with a formation, either in open hole or through perforations in the casing. By squeezing cement at given depths (1) hydrocarbon producing zones can be segregated from those formations producing other fluids, (2) casing leaks can be repaired or, (3) thief zones sealed. In oil-field practices cement is exposed to an infinite variety of environments; therefore, cements with various qualities are needed. To provide for these growing needs the American Petroleum Institute annually produces a list of cements, API Standards 10A, Specifications for Oil-Cements and Cement Additives for manufactures and users. They are listed in the API Standards 10A dated April 1977 as follows:
Class A: Intended for use from surface to 6,000 ft (1830 m) depth when special properties are not required. Available only in ordinary type. Class B: Intended for use from surface to 6,000 ft (1830 m) depth when conditions require moderate to high sulfate-resistance. Available in both moderate and high sulfate-resistant types. Class C: Intended for use from surface to 6,000 ft (1830 m) depth when conditions require high early strength. Available in ordinary and moderate and high sulfate-resistant types. Class D: Intended for use from 6,000 ft to 10,000 ft (1830 m to 3050 m) depth under

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conditions of moderately high temperatures and pressures. Available in both moderate and high sulfate-resistance types.
Class E: Intended for use from 10,000 ft to 14,000 ft (3050 m to 4270 m) depth under conditions of high temperatures and pressures. Available in both moderate and high sulfateresistant types. Class F: Intended for use from 10,000 ft to 16,000 ft (3050 m to 4880 m) depth under conditions of extremely high temperatures and pressures. Available in both moderate and high sulfate-resistant types. Class G: Intended for use as a basic cement from surface to 8,000 ft (2440 m) depth as manufactured, or can be used with accelerators and retarders to cover a wide range of well depths and temperatures. No additions other than calcium sulfate or water, or both, shall be interground or blended with the clinker during manufacture of Class G cement. Available in moderate and high sulfate-resistance types. Class H: Intended for use as a basic cement from surface to 8,000 ft (2440 m) depth as manufactured, and can be used with accelerators and retarders to cover a wide range of well depths and temperatures. No addition other than calcium sulfate or water, or both, shall be interground or blended with the clinker during manufacture of Class H cement. Available in moderate and high (Tentative) sulfate-resistant types. Class J: Intended for use as manufactured from 12,000 ft to 16,000 ft (3650 m to 4880 m) depth under conditions of extremely high temperatures and pressures or can be used with accelerators and retarders to cover a range of well depths and temperatures. No additions of retarder other than calcium sulfate, or water, or both, shall be interground or blended with the clinker during manufacture of Class J cement.

Although the API lists nine different classes of cement, only five (A, B, C, G, H) are available from manufacturers in the United States. These five cements with the addition of chemicals called additives (see Appendix B) can change cement properties to meet most well conditions. Class G and H cements are very similar and are the most commonly used. G is used in California and H in the Gulf Coast Areas. As in our discussion of drilling fluids, we will first examine field test that evaluates critical properties of oil field cements. These tests are outlined for standardization in API RP 10B. Then, several experiments are presented to expose the student to the measurement of such properties as compressive strength, thickening time, etc. and their role in providing adequate cement control.

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TEST PROCEDURES
WATER CONTENT OF SLURRY

Water is added to cement to make the slurry pumpable and provide for hydration (the chemical reaction), although only 25.0 % water by weight of cement may be needed for hydration, normal water content is higher to provide for pumpability. Minimum and maximum water content values are determined for given cement in the following manner.
Minimum Water Content

The minimum amount of water for any class of cement is defined as that amount of which can be used without producing a slurry of consistency greater than 3O Uc2 as measured by a consistometer (the consistometer operation is described in the section labeled Thickening Time). If less than the minimum amount of water is used, the friction in the annulus plus the hydrostatic pressure may be high enough to break down weak formations. In addition, since the watercement ratio is low, the loss of a small amount of water to thief zones or tubing leaks may cause the cement to set prematurely. On the other hand, it may be necessary to use the minimum water content where maximum slurry weight or strength is required or to control lost circulation.
*All cement additives are given as a percent of the dry cement weight. Procedure:

1. The required quantity of water shall be placed in the Waring blender at slow speed and the cement sample added. 2. After all the cement has been added to the water, cover the container and stir at high speed for 35 seconds. 3. Pour the slurry immediately into the atmospheric consistometer and stir at 80F for a period of 20 minutes, at which time the consistency shall be recorded. 4. Several runs with various water contents should be made and plotted to determine the amount of water at which a consistency of 30 Uc is obtained and, therefore, the minimum water content.
Maximum Water Content

The maximum water content is defined as that quantity of water that can be mixed with a given cement without causing the separation of more than 2.5 ml of free-floating water when the slurry is allowed to stand for 2 hours at room temperature in a 250 ml graduate. If more than the maximum amount of water is used, cement particles will settle out of the slurry to the extent that free-water pockets and low-strength cement will exist within the cement column. The maximum
2

Universal consistency units (Uc) are dimensionless units formerly referred to as poises.

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water content should never be exceeded unless bentonite gel or a similar material is blended with the cement to tie up excess water.
Procedure:

1. Prepare cement slurry as previously described. 2. Pour the slurry immediately into an atmospheric consistometer and stir at 80 F for 20 minutes. 3. Then remix the slurry an additional 35 seconds at high speed. 4. Fill a 250 ml graduate cylinder with slurry, seal with a rubber stopper, and let stand for 2 hours. 5. Remove the supernatant water developed by standing with a pipette and measure in a graduated cylinder. 6. Several runs with various water contents should be made and plotted to determine which water content yields 2.5 ml of free water on standing 2 hours. This is the maximum water content for the tested cement.

DENSITY

The density of cement slurry is, except for squeeze jobs, slightly heavier than the mud in the hole. This minimizes chances of either a blowout or lost circulation occurring during cementing and aids in removing drilling mud from the hole. The density can be controlled by the amount of water (between minimum and maximum stated above) added to the slurry. In addition, for lower densities -10.8 to 16.5 lb/gal, materials that hold large volumes of water such as bentonite, diatomaceous earth or expanded perlite are often used. For greater densities 15.6 to 22 lb/gal, weighting materials such as hematite and barite are commonly used. In field operations, slurry density is customarily monitored with a standard mud balance. Automated weighting devices, however, fitted into the discharge line between the mixing unit and the wellhead, give a more uniform weight record and are becoming an accepted practice.
Mud Balance

The Mud Balance provides a simple method for the accurate determination of mud density. Durably constructed, it consists principally of a base and graduated arm with cup, lid, knife edge, rider, level, and counterweight.

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Procedure:

1. Remove lid and fill cup to the top with sample to be tested. Puddle the sample 25 times with a glass rod to remove entrapped air. 2. Replace lid and rotate until firmly seated, making sure some sample squeezes out the vent hole. 3. Wipe sample from exterior of balance. 4. Place balance on base with knife edges on fulcrum rest. 5. Move rider until instrument is in balance, as determined by level. 6. Read sample density at end of rider nearest fulcrum.
Results:

The instrument must first be calibrated by using distilled water as the sample. After measuring the density of the water, dry the cup and then measure the density of the mud. Calculate the true mud density (corrected for balance error) using the following formula: Measured density of distilled water Measured mud density = True density of distilled water True mud density The density of distilled water is 8.33 pounds/gallon or 62.4 pounds/cubic foot. (Alternately, balance error of the Mud Balance can be eliminated by adding or removing lead shot from the counterweight.)

STRENGTH TESTS

One major performance criterion of oil-well cement is in its strength. Cement must (1) secure and support easing in the hole, (2) set quickly to reduce rig waiting on cement (WOC) time, and (3) withstand the shock of continued drilling and perforating. There is no universal agreement on strength requirements for oil-well cements; however, it is generally accepted in the industry that a compressive strength of 500 psi is adequate for most operations. Three variables - cement type, temperature, and pressure - affect the setting time and ultimate compressive strength. Since temperature and pressure of the well are predetermined we must alter the cements composition to minimize WOC time yet provide adequate strength. Early strength is increased with the addition of accelerators such as calcium chloride, ammonium chloride and minimum water. In hot or high pressure formations it may be useful to retard the cements setting time with lignosulfonate, CMHEC, and maximum water. But also in high temperature formations, cement compositions may retrogress (lose strength) after reaching a high value.

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Cements containing retarders for high temperature applications seem particularly subject to strength retrogression. Although remaining compressive strength may be adequate for many applications, the addition of 35% silica flour to the slurry provides a way to maintain compressive strength.
Versa Tester

The Versa Tester is a hydraulic loading apparatus which compresses cement specimens until they fail (fracture). Unlike the machines used in sophisticated testing which load specimens mechanically at a constant rate (1000-4000 psi/min) you must hand load specimens in the Versa Tester. When adding pressure to your specimens take care to load the samples slowly. Also note that reliable strength tests depend upon careful observance of all specified requirements and procedures. Improper centering of specimens in the Versa Tester can result in oblique fractures yielding low-strength results.
Procedure: 3

1. Prepare the cement slurry to be tested as previously described. 2. Place the slurry in the lightly greased molds and puddle each mold.25 times. 3. After pudding, remove the excess slurry from the top of each mold using a straightedge. 4. Specimens can be cured at atmospheric temperature or in an oven for periods of 8, 24, 48 and 72 hours. 5. When samples are to be tested at ages of less than 24 hours, remove the samples from the oven approximately 30 minutes before testing. 6. Set the sample to be tested on the Versa Tester platform centered under the hydraulic piston. 7. Close the valve on the hydraulic pump and lower the piston onto the sample. 8. Add pressure slowly onto the sample by pumping and record the maximum pressure. Have another person watch the gauge as you load the sample. (It will return to 0 pounds when the sample fails). Note: the gauge reads pounds and you must convert to psi by dividing by the average cement cross-sectional area. Average area =
Results:

1 (Area of bottom + Area of top ) 2

The compressive strength (psi) of the sample tested is measured as the maximum pressure prior to failure on the Versa Tester. Strengths of 500 psi are normally necessary prior to returning to drilling operations. By measuring strengths at various times the WOC can be estimated.
3

Always wear eye protection when testing cements compressive strength.

21

THICKENNING TIME

Cement slurry must remain pumpable until it is in place, within some margin of error. This limit of pumpability i.e. thickening time is defined as when the slurry reaches a viscosity of 100 poises. Thickening time is a function of both temperature and pressure as shown below. It must be established to ensure adequate pumping time for slurry placement. Avoid cements with excessive thickening times to prevent; delays in resuming drilling operations, settling and separation of cement slurry components, formation of free-water, pockets, loss of hydrostatic head and gas cutting.
Consistometer

Thickening time is measured using a pressurized or atmospheric (our model) consistometer. As the apparatus applies heat and pressure to the slurry, simulating cement flow in a well, a continuous consistency measurement is recorded as a strip chart. The limit of pumpability is reached when the torque on the paddle in the slurry cup reaches 100 Uc. Please note that these measurements are made in metal vessels which prevent any fluid loss. Your time valves will be higher than they might be opposite a permeable zone, after partial dehydration.
Procedure:

Care shall be taken to see that the apparatus is clean. After each test the inside of the cell and the paddles, particularly the outside edges should be cleaned and brushed. Surfaces that come in contact with the slurry shall be given a thin coating of waterproof grease or light oil before each test. 1. Fill the bath with water. Place the empty cells in the water bath and bring the bath to the testing temperature. After the bath has reached this temperature set the heat control and turn the switch to low. 2. Test the paddle for excessive friction by running the cylinder assembled, but without cement inside, for a few minutes. If the paddle is bent to such an extent that it rubs on the side, an appreciable movement will be shown by the indicator. The two bearings in the slurry indicating lid should be checked periodically for excessive friction. These defects, if found, should be corrected before starting additional tests. 3. With the paddle out, fill each cylinder of the consistometer with 500 cc (the line scribed the cylinder). Some space has been left between the scribed line the lid for increased volume when the paddle is inserted in the cylinder and when the slurry is heated. The slurry is poured into the cylinder, the paddle inserted, and the lid put on, being careful that the slotted shaft engages the pin in the lid, The cylinder is then placed in the consistometer, and the viscosity (Uc) is read on the scale. The scale is divided into 10 units, with each division representing 10 Units of Consistency. A reading of 3 would be 30 Units of Slurry Consistency, etc. 22

4. Start the motor and a stop watch and take readings every 10 minutes for the first hour and at every 30 minutes thereafter until the cement starts to stiffen. 5. When either sample has reached a consistency of 70 Uc, turn off the motor and remove the cylinder for cleaning, if the other cement slurry has not started to set, the test may be continued with only one cell in place.
6. BE CERTAIN THAT EACH CELL IS CLEANED IMMEDIATELY AFTER IT IS REMOVED.

Observe the following precautions: 1. Watch the indicators during a test run. Do not allow the cement to remain in the containers after a consistency of 10 has been reached. 2. Check and clean the bearings before each test. 3. Watch the temperature control. 4. Never turn the heater on unless the bath is fitted with water. 5. Cover the water surface with a film of oil to prevent rusting. 6. Do not mix parts. Each container is a separate unit. 7. Remove the cement immediately after removing the cylinder. 8. Never use force or pry the gears when placing a cylinder. 9. Do not clean the cylinders or paddles with acid. 10. Slide the cylinder bracket out, place the cylinder, and push forward to engage the gears. 11. Be sure that the end of the thermometer is submerged. 12. Be sure that the pointers read zero before starting the test. 13. Be sure that the indicator cord lies on the outside circumference of the cylinder top.
Results:

The results of tests are read directly from the indicator and no calculations are necessary so long as the machine is in calibration. However, the consistency readings may be plotted on common graph paper with the consistency as the ordinate and time as the abscissa. The general shape of the consistency-time curve plotted as described above presents an excellent picture of a particular cement as far as its setting characteristics are concerned. A visual comparison of the curves of several cements will usually disclose characteristic differences with regard to a particular cementing application. There are certain features common to all consistency-time curves. The cement slurry generally has a fairly low initial consistency. As stirring is continued, this value usually drops a little more. It then begins to increase at very gradual rate. However, as time goes on, the rate of 23

increase of consistency is accelerated to such an extent that the latter part of the curve is quite steep. This acceleration varies with different cements and with different testing temperatures. From the standpoint of the majority of oil-well cementing requirements, a proper cement slurry should reveal the following characteristics on a consistency curve produced with a Halliburton Consistometer at temperatures corresponding to well conditions. 1. Initial consistency between 10 and 30 Uc (Units of Consistency) 2. Consistency to remain below 40 Uc for 3 hours from time of introductions into consistometer. 3. Sharp break toward higher consistency after 3 hours. 4. Tangent to curve should be practically vertical when curve reaches consistency of 100 Uc. This feature is indicative of the rapidity with which the cement will develop strength after initial set.
Note:

It is understood that units of measurement of viscosity should properly apply only to true fluids, and that a cement slurry is not a true fluid; however, the effective resistance to flow offered by a cement slurry can be conveniently measured by a Halliburton Consistometer and, hence, the advantage of expressing the consistency of a cement slurry in terms of Units of Consistency (Uc)

FLUID LOSS

The water loss of neat cement is extremely high. Consequently, when a slurry contacts a porous formation from which the mud cake has been removed, it may quickly become dehydrated and undergo a flash set. This problem is common in cementing deep liners and in squeeze cementing. In the 1960s, significant progress was made in developing cement additives that lower fluid loss with a high molecular weight, synthetic polymer but these additives are usually affected by temperature. Generally, thickening time is retarded and, at low temperature, this retardation may have to be offset by accelerators. Bentonite and CMHEC are also used to reduce filtrate loss.
Cement Filter Press

To measure filtrate characteristics of cement slurries, the API specifies a standardized 30minute test at 100 psi. The API procedure employs a filter assembly consisting of a frame, a cylinder, and a 325mesh screen supported by a 60-mesh screen as the filtration medium. The heating jacket makes it possible to simulate formation temperatures. 24

Procedure:

1. The filter press cylinder shall be filled with the cement to be tested, capped, and secured in the frame. 2. Place a dry graduated cylinder under the drain tube to receive the filtrate. 3. Close the relief valve and pressure the system to 100 psi with the gas supplied. 4. Timed from the initial pressure application, filtrate readings shall be taken at , , 1, 2, and 5 minutes and thereafter at 5-minutes intervals until 30 minutes have elapsed. 5. If dehydration occurs before the end of the 30-minutes test period, the time required to dehydrate the sample shall be observed. 6. Release the pressure on the filter pressure and clean with water making sure the screen is properly washed.
Results:

The API filter loss of all cement slurries without additives is high-in excess of 1,000 ml. When all the filtrate is received in the test cell in less than 30 minutes, the following equation is used to calculate the hypothetical 30-minute fluid-loss valve. F30 = Ft where 5.477 t

F30 = quantity of filtrate in 30 minutes Ft = quantity of filtrate at time t. t = time in minutes

Cement slurries having laboratory fluid-loss values of 50 to 150 ml in 30 minutes are commonly used in squeeze cementing. In cementing deep liners, the API filter loss may be as high as 300 ml.

PERMEABILITY

Although in designing cement slurries only slight emphasis is given to the permeability of set cement, there are means of measuring it for both water and gas. The API has specified a standard system that involves the use of a permeameter, which we will not use in this course. Set cements have very low permeabilities - much lower, in fact, than those of most producing formations. Data have shown that at temperatures less than 200 F the permeability of cement decreases with age and temperature. After 7 days of curing, the permeability is usually too low to measure. The permeability of set cement to gas is normally higher than to water, but measurements of 25

the former are less reliable because it is difficult to obtain good representative samples for measuring gas flow. Cements that have set for 3 to 7 days have a gas permeability of less than 0.1 md. Dolomite and limestone have an average of 2 to 3 md and oolitic limestones usually have a very low permeability. Sandstone has gas permeability ranging from 0.1 to 2,000 md. Silica flour, besides inhibiting strength retrogression, also reduces the permeability of set cements. For example, cements cured at 350 F displayed a permeability of 1 md but with the addition of 35% silica flour was reduced to less than 0.001 md.

RHEOLOGICAL PROPERTIES

A common cause of failure in primary cementing is incomplete displacement of drilling muds, which can leave vertical, mud filled channels of cement. This mud may be displaced later under producing conditions to create open channels that permit formation fluids to migrate upward behind the casing. Two basic forces are associated with drilling and displacement during primary cementing. They are differential pressure and cement-on-mud (fluid-on-fluid) drag forces. To effectively displace muds, oil well cements must exert a combination of differential pressure and drag forces of sufficient magnitude to overcome forces resisting displacement. Mud and oil well cement slurries being non-Newtonian in nature (viscosity changes with shear rate) has led to several mathematical models beings used in predicting flow properties and interrelationships of such muds and cements. The Bingham Plastic Model and the Power Law Model are most commonly used. The former has been utilized since the mid-1940s, power Law Model Equations - presented in the late 1950s - are more generally used than those of the Bingham Model and will be presented here. Such models attempt to describe the relationship of shear rate and shear stress for muds and slurries. Extremely useful in analyzing the displacement process, they are not precise techniques and should be used only as an indicator to acceptable displacement conditions.
Baroid Rheometer

The Baroid Rheometer is used to measure the consistency index (K) and flow behavior index (n) of cements. Field models have two speeds to develop shear rate to 300 and 600 rpm, while our lab model has constant variation from 0 to 600 rpm.
Procedure:

1. Prepare the prescribed slurry in the Waring Blender in accordance with the previous procedure described in the section titled Minimum Water Content. 2. The cement shall then be stirred at slow speed for a period of 10 minutes. 3. Transfer slurry to sample cup with minimum time lag. With rotor turning at 600 rpm,

26

place rotor into the cup containing the slurry up to the level at the designated line on the sleeve. 4. The initial reading at 600 rpm shall be taken 60 seconds after continuous rotation. Then lower the rotor speed to 300 rpm, rotate for 60 seconds and read. Remove the sample and clean rheometer with water.
Results:

The pressure at any point in the well bore is the sum of the hydrostatic pressure and the frictional pressure. The hydrostatic pressure is the pressure exerted on the formations, casings, and down-hole equipment by the weight of the fluid or fluids above them, Friction pressure is generated by the resistance of the fluids to the movement. P = Ph + Pf where: P = Total pressure at any point in the well bore Ph = hydrostatic pressure Pf = friction pressure

The hydrostatic pressure is: Ph = 0.052 L Where: Ph = hydrostatic pressure, psi = fluid density, lb/gal L = length of the fluid column, ft (vertical depth)

The friction pressure is not easy to calculate since it depends on the rheological behavior of the fluid as it is exposed to shear caused by pumping. For general purposes, the following calculation approach to friction pressure is perhaps appropriate. It assumes that the cement slurry behaves as a power-law fluid. Calculate the flow-characteristic parameters by using the equations: N = (3.32) log10 (600-rpm reading/300-rpm reading) K = (1.0660 (300-rpm reading)/[(100) (511)n] To determine friction pressure, calculate the Reynolds number, NRe, from the following equations: For annulus: NRe = (547) (dw do)n (Q)2-n ( )/[(1,647)n (dw2 do2)2-n (K)] For casing: NRe = (547) (Q)2-n ( )/[(1 ,647)n (di)4-3n (K)] where Q = Pumping rate, bbl/min = Fluid density, lb/gal di = Casing ID, in. 27

dw = Hole diameter, in. do = Casing OD, in. Nre = Reynolds number, dimensionless. Using the n-valve and Reynolds number, estimate a friction factor from the figure above. Friction pressure is then determined by: For casing: Pfc = (11.5) (L) ( ) (Q2) (f)/di5 For annulus: Pfa = (11.5) (L) ( ) (Q2) (f)/[dw-do) (dw2 do2)2] where: f = Friction factor, dimensionless Pfc = Friction pressure in casing, psi Pfa = Friction pressure in annulus, psi

Notice that the above calculations must be performed for every fluid using the corresponding n, K, and . Also, the Ls will be different for each both inside and outside the casing.
Pressure: Once all the individual hydrostatic and friction pressures are calculated for each fluid in the casing and annulus, the total hydrostatic and frictional pressures for the casing and annulus can be calculated by simple addition. Next, the surface and bottom-hole pressures can be calculated:

Ps = Pf + Pa - Pc PB = Pfa + Pa where: Ps = Surface pumping pressure, psi. PB = Bottom hole, circulating pressure, psi Pa = Total hydrostatic pressure in annulus, psi Pc = Total hydrostatic pressure in casing, psi Pf = Total friction pressure (casing and annulus), psi

Hydraulic horsepower: The following equation can be used to calculate the hydraulic horsepower needed to circulate the well at the given rate:

Hhp = 0.0245 (Ps) (Q) where: Hhp = Hydraulic horsepower Ps = Surface pumping pressure, psi Q = Pump rate, bbl/min

Turbulent flow rate: Cement placement under turbulent flow conditions is an effective technique for achieving a good cement job. The pumping rate for turbulent flow may be determined from the following procedure.

28

First, determine n and k for the cement slurry as outlined above. Then determine the upper critical Reynolds number for turbulent flow, from the friction-factor chart (notice that the upper critical Reynolds number changes with n, and varies from about 2,900 to 3,500. A good average number is 3,000). Calculate the turbulent flow rate from the equation: Q2-n = (NRe) (1,647)n (dw2 do2)2-n (k)/[(547) (dw do)n ( )] Where: Q = Flow rate, bbl/min NRe = Reynolds number, dimensionless n = Fluid-flow behavior index, dimensionless K = Fluid consistency index, lb-sec/sq ft dw = Diameter of well bore, in. do = 0D of casing, in

The value obtained for Q is the minimum rate at which the cement must be pumped to achieve turbulent flow.

29

FIELD TESTING OF DRILLING FLUIDS Laboratory Experiment No. 1 Properties of Fresh Water Muds
Object:

Become familiar with the mud testing apparatus and procedures by investigating the properties of fresh water muds.
Theory:

Certain clay mineral, when ground to colloidal size and contacted with water, readily hydrate (adsorb water) to form stable colloids. Different clay minerals have different abilities to adsorb water. The more water adsorbed by the clay, the higher the viscosity of the resulting mud will be. In general, simple water-clay systems are suitable for shallow or upper hole drilling in areas where contaminating beds are not a problem. Unfortunately, fresh water muds are easily subject to contamination and the muds develop objectionable properties (as we shall see in later experiments).
Procedure:

Each group of the lab section will test different drilling mud clays. Description of clay types is included in Appendix A. The lab instructor will prepare the muds for you in the following manner: 1. Add the required amount of clay to the required amount of fresh (distilled) water. 2. Stir 10 minutes with the mixer 3. Age the mud overnight.
GROUP 1 2 3 MUD NAME Aquagel* Zeogel* Quick-Gel* MUD 1 (gr. clay/cc water) 50/1000 50/1000 25/1000 MUD 2 (gr. clay/cc water) 100/1000 100/1000 50/1000

*These materials are Baroid trade names. Their functions are described in Appendix A. Each group will test their two muds for the following properties using the equipment and procedures described in the previous section: 1. Density (Mud Balance). 2. Marsh Funnel viscosity (Marsh Funnel). 3. Apparent viscosity, plastic viscosity, yield point, 10-sec gel strength, 10-min gel strength (Baroid Rheometer). 30

4. Fluid loss, mud cake thickness (Filter Press). 5. pH (Litmus Paper). 6. Mud, mud filtrate, and mud cake resistivity (Resistivity Meter).
Note the following:

1. Blend mud for 5 minutes before making first test. 2. Return the sample to the sample container after measuring each property EXCEPT fluid loss and re-stir it by hand. 3. Perform the fluid loss test LAST. 4. For Mud 1, do complete 30-min filtration test. For Mud 2, do a 7.5-min filtration test and report the corrected 30-min loss.
Results:

1) Tabulate the following mud properties: a) Mud density (ppg). b) Apparent viscosity (cp) @ 10, 50, 100, 200, 300, and 600 RPM. c) Plastic viscosity (cp). d) Yield point (lbs/100 sq. ft.). e) 10-sec gel strength (lbs/100 sq. ft.). f) 10-min gel strength (lbs/100 sq. ft.). g) pH. h) Corrected 30-min fluid loss (ml). i) Filter cake thickness (in.). j) Mud resistivity (ohm-m). k) Mud filtrate resistivity (ohm-m). l) Mud cake resistivity (ohm-m). 2) Plot the following mud properties vs. % of clay in the mud: a) Mud density (ppg). b) Hastic viscosity (cp). c) Yield point (lbs/l00 sq.ft.). d) 10-min gel strength (lbs/100 sq.ft.). e) Corrected 30-min fluid loss (ml). 3) Summarize the results of doing the following experiments: a) Increasing the concentration of general purpose bentonite clay in a fresh water-based mud (Group 1). b) Increasing the concentration of high-yield bentonite clay in a fresh water-based mud (Group 2). c) Increasing the concentration of attapulgite clay in a fresh water-based mud (Group 3). 4) Compare the results of using general purpose bentonite clay, high-yield bentonite clay, and attapulgite clay to build a fresh water-based mud.

31

FIELD TESTING OF DRILLING FLUIDS Laboratory Experiment No. 2 Effects of Sodium Salts on Fresh Water Muds
Object:

To investigate the effects of salt on fresh water muds and to evaluate aids in overcoming the adverse effects caused by salt contamination.
Theory:

Clay particles dispersed in water are in the form of sheets which possess electrical charges (unsatisfied valences). The presence of these charges gives fresh water muds their excellent viscous, thixotropic, and filtration properties. Salt concentrations, however, neutralize the electric charges and cause flocculation (formation of particle aggregates which are larger than colloidal size) of the clay particles. As a result, the mud may be valueless for its usual functions. Salt contamination can be due to two different factors, each having different effects on the mud. First, formations containing salt water are frequently encountered in the drilling of wells. If the mud weight is too low, salt water intrusion may occur with adverse effects on the mud viscosity. In some wells salt formations are encountered either as beds or salt plugs. Second, salt contamination may be due to the presence of salt in the water used to mix the mud (especially true when sea water is used). Whatever the reason, contamination of mud by salt is a frequent phenomenon and the full effect of this compound is of considerable importance.
Procedure:

Your lab instructor has prepared the muds for you in the following manner:
Group 1 Mud 1: Add 50.0 gr. of Aquagel to 1000.0 cc of water, stir with mixer for 10 minutes, age mud overnight. Mud 2: Dissolve 10.0 gr. of sodium chloride (NaCl) in 990.0 cc of water to make a 1.0 % salt solution, add 50.0 gr. of Aquagel and stir with mixer for 10 minutes. Age mud overnight. Mud 3: Dissolve 50.0 gr. of NaCl in 950.0 cc of water to make a 5.0 % salt solution, add 50.0 gr. of Aquagel. Proceed as in Mud 2/Group 1. Mud 4: Dissolve 150 gr. of NaCl in 850 cc of water to make a 15.0 % salt solution. Add 50.0 gr. of Aquagel. Proceed as in Mud 2/Group 1.

32

Group 2 Mud 1: Same as Mud 1/Group 1. Mud 2: Add 50.0 gr. Aquagel to 990.0 cc of water, stir with mixer for 10 minutes. Add 10.0 gr. of sodium chloride (NaC1) and stir with mixer for 10 minutes. Age mud overnight. Mud 3: Proceed as in Mud 2/Group 2 but use 50.0 gr. of Aquagel, 950.0 cc of water and 50.0 gr. of NaC1. Mud 4: Proceed as in Mud 2/Group 2 but use 50.0 gr. of Aquagel, 850.0 cc of water and 150 gr. of NaCl. Group 3 Mud 1: Same as Mud 1/Group 1. Mud 2: Dissolve 50.0 gr. of sodium chloride (NaC1) in 950.0 cc of water to make a 5.0 % salt solution. Add 50.0 gr. of Aquagel, 6.0 gr. of Q-Broxin* and stir with mixer for 10 minutes. Age mud overnight. Mud 3: Proceed as in Mud 2/Group 3 but use 50.0 gr. of NaCl, 950.0 cc of water, 50.0 gr. of Aquagel and 6.0 gr. of Impermex*. Mud 4: Proceed as in Mud 2/Group 3 but use 50.0 gr. of NaCl, 950.0 cc of water, 50.0 gr. of Aquagel and 6.0 gr. of Loloss*.

*Description included in Appendix A. Each group will test their 4 muds for the following properties: 1. Density (Mud Balance). 2. Apparent viscosity, plastic viscosity, yield point, 10-sec gel strength, 10-min gel strength (Baroid Rheometer). 3. Fluid loss, mud cake thickness (Filter Press). 4. pH (Litmus Paper). 5. Mud, mud filtrate, and mud cake resistivity (Resistivity Meter).
Note the following:

1. 2. 3. 4.

Blend mud for 5 minutes before making first test. Return the sample to the sample container after each test and re-stir it by hand. Perform the fluid loss test LAST. Do a 7.5-min filtration test and report the corrected 30-min loss.

33

Results:

1) Tabulate the following mud properties: a) Mud density (ppg). b) Plastic viscosity (cp). c) Yield point (lbs/100 sq. ft.). d) 10-sec gel strength (lbs/100 sq. ft.). e) 10-min gel strength (lbs/100 sq. ft.). f) pH. g) Corrected 30-min fluid loss (ml). h) Filter cake thickness (in.). i) Mud resistivity (ohm-m). j) Mud filtrate resistivity (ohm-m). 2) Plot the following mud properties vs. % of NaCl (Group 1), % of NaCl (Group 2), and % of Additive (Group 3): a) Plastic viscosity (cp) b) Yield point (lbs/l00 sq. ft.). c) 10-sec gel strength (lbs/l00 sq. ft.). d) 10-min gel strength (lbs/100 sq.ft.). e) Corrected 30-min fluid loss (ml). f) Mud resistivity (ohm-m) g) Mud filtrate resistivity (ohm-m) 3) Summarize the results of doing the following experiments: a) Increasing the salt contamination of fresh water muds due to salt in the mixing water (Group 1). b) Increasing the salt contamination of fresh water muds due to salt encountered in the borehole (Group 2). c) Adding viscosity and filtration control agents to salt contaminated mud (Group 3). 4) Compare the results of salt contamination in fresh water muds due to salt in the mixing water due to salt encountered in the borehole.

34

FIELD TESTING OF DRILLING FLUIDS Laboratory Experiment No. 3 Viscosity Reducing Agents
Object:

Evaluate the performance of several mud thinners.

Theory:

Viscosity reducing agents are necessary to the handling of water-based muds. Fresh waterbased muds normally contain bentonite clay for the purpose of developing desirable viscous and low fluid loss properties. High concentrations of clay compounds, other low-specific-gravity solids such as drill cuttings, or soluble salts may be responsible for undesirable mud viscosity, gel strength, and fluid loss in fresh water-based mud systems. The problem of calcium contamination can frequently be handled successfully through the use of chemical agents who precipitate the contaminant and restore satisfactory properties to the mud. High viscosity, gel strength, and fluid loss caused by non-precipitable salts such as NaCl or by excess concentrations of solids may be treated by diluting the mud with water (reduces both salt and solids concentrations) or by mechanical methods (reduces solids concentration only). These actions, however, also result in a decrease in both the Bentonite concentration and mud weight. Therefore, Bentonite usually has to be added back to the mud to restore desired rheological and fluid loss properties and weighting material usually has to be added back to the mud to restore required density. Such treatment is often unsatisfactory or uneconomical and other means are frequently used to obtain a reduction in viscosity, gel strength, and fluid loss without requiring the supplementary use of Bentonite and weighting material. An alternative to water dilution and mechanical separation is treatment with viscosity reducing agents. A viscosity reducing agent, usually very expensive, may be defined as any additive to water-based muds capable of reducing viscosity and gel strength by means other than dilution or precipitation of the agent responsible for the abnormal viscosity. This definition eliminates water as a viscosity reducer although it is frequently the most advantageous and the least expensive agent to use and is sometimes the only additive which will give the required effect. This definition also eliminates such compounds as sodium bicarbonate, soda ash, barium carbonate, etc., which all reduce mud viscosity by precipitating calcium or by regulating the mud pH. The chemicals which have been found effective as viscosity reducers consist of a relatively narrow set of compounds. Practically, they are the molecularly dehydrated phosphates and polyphosphates, the plant tannins, the lignosulfonate wood by-products, and the mineral lignins. The ability of viscosity reducers is strictly limited and their addition to the mud above the low concentrations required for particle saturation will not result in further viscosity reduction. In 35

fact, often the reserve is true and viscosity increases.

Procedure:

Your lab instructor has prepared the muds for you in the following manner:
Group 1 Mud 1: Add 50.0 gr. of Aquagel to 600.0 cc of water and stir with mixer for 10 minutes. Age mud overnight. Mud 2: Add 50.0 gr. of Aquagel to 600.0 cc of water, stir with mixer for 10 minutes. Add 0.4 gr. of CC-16* and stir with mixer for 10 minutes. Age mud overnight. Mud 3: Proceed as in Mud 2/Group 1 but use 1.0 gr. of CC-16. Mud 4: Proceed as in Mud 2/Group 1 but use 4.0 gr. of CC-16. Group 2 Mud 1: Same as Mud 1/Group 1. Mud 2: Proceed as in Mud 2/Group 1 but use 0.4 gr. of Barafos* instead of CC-16. Mud 3: Proceed as in Mud 3/Group 1 but use 1.0 gr. of Barafos instead of CC-16. Mud 4: Proceed as in Mud 4/Group 1 but use 4.0 gr. of Barafos instead of CC-16. Group 3 Mud 1: Same as Mud 1/Group 1. Mud 2: Proceed as in Mud 2/Group 1 but use 0.15 gr. of SAPP* instead of CC-16. Mud 3: Proceed as in Mud 3/Group 1 but use 0.25 gr. of SAPP instead of CC-16. Mud 4: Proceed as in Mud 4/Group 1 but use 0.30 gr. of SAPP instead of CC-16.

*Description included in Appendix A. Each group will test their 4 muds for the following properties: 1. Density (Mud Balance). 2. Plastic viscosity, yield point, 10-sec gel strength, 10-min gel strength (Baroid Rheometer). 3. Fluid loss (Filter Press). 4. pH (Litmus Paper).
Note the following:

1. 2. 3. 4.

Blend mud for 5 minutes before making first test. Return the sample to the sample container after each test and re-stir it by hand. Perform the fluid loss test LAST. Do a 7.5-min filtration test and report the corrected 30-min loss. 36

Results:

1) Tabulate the following mud properties: a) Mud density (ppg). b) Plastic viscosity (cp). c) Yield point (lbs/100 sq. ft.). d) 10-sec gel strength (lbs/100 sq. ft.). e) 10-min gel strength (lbs/100 sq. ft.). f) pH. g) Corrected 30-min fluid loss (ml). 2) Plot the following mud properties vs. % of thinner in the mud: a) Plastic viscosity (cp) b) Yield point (lbs/l00 sq. ft.). c) 10-sec gel strength (lbs/l00 sq. ft.). d) 10-min gel strength (lbs/100 sq. ft.). e) Corrected 30-min fluid loss (ml). 3) Summarize the results of doing the following experiments: a) Increasing the concentration of the thinner CC-16 in a fresh water-based mud (Group 1). b) Increasing the concentration of the thinner Barafos in a fresh water-based mud (Group 2). c) Increasing the concentration of the thinner SAPP in a fresh water-based mud (Group 3). 4) Compare the results of adding the thinners CC-16, Barafos, and SAPP to a fresh water-based mud.

37

FIELD TESTING OF DRILLING FLUIDS Laboratory Experiment No. 4 High Temperature Effects
Object:

Evaluate the effects of high temperature on drilling muds.

Theory:

The filtration properties of drilling mud are a measure of the ability of the solid components of the mud to form a thin, low-permeability filter-cake. The lower the permeability, the thinner the filter cake and the lower the volume of filtrates from mud of comparable solids concentration. This property is dependent upon the amount and physical state of the colloidal material in the mud. It has been shown repeatedly in the filed that when mud of sufficient colloidal content is used, drilling difficulties are minimized. In contrast a mud low in colloids and high in inert solids deposits a thick filter cake on the walls of the hole. A thick filter cake restricts the passage of tools and allows an excessive amount of filtrate to pass into the formation, thus providing a potential result in further trouble such as difficulty in running casing, creating a swabbing effect which may cause the formation to cave or swab reservoir contents into the hole, and difficulty in securing a water shutoff because of channeling of cement. In previous laboratories the filtration properties of drilling mud were tested at a specified pressure of 100 psig, and room temperature. In this laboratory the filtration properties of a drilling mud will be tested at high temperatures as may be encountered at the bottom of the hole.
Procedure:

Each group of the lab section will test different mud clays. Description of each of the clays is included in Appendix A. The lab instructor will prepare the muds for you in the following manner: 1. Add the required amount of clay to the required amount of fresh (distilled) water. 2. Stir 10 minutes with the mixer 3. Age the mud overnight.
GROUP 1 2 3 MUD NAME Aguagel* Zeogel* Quick-Gel* MUD 1 (gr. clay/cc water) 50/1000 50/1000 25/1000 MUD 2 (gr. clay/cc water) 100/1000 100/1000 50/1000

*These materials are Baroid trade names. Their functions are described in Appendix A. 38

Each group will test their muds at two temperatures according to the following manner:
A. Preheating the Heating Jacket

1. Connect the power cord to the proper line voltage as indicated on the nameplate. 2. Turn the thermostat to near mid-scale. 3. Place the metal stem dial thermometer in the thermometer well of the heating jacket. 4. The pilot light will turn on when the heating jacket temperature has reached the thermostat setting. 5. Readjust the thermostat as necessary to obtain the desired test temperature. (Just below 3 is 200 F.)
B. Loading the Filtration Cell

***SAFETY NOTE***. The filtration Cell Assembly constitutes a Pressure Vessel. The SAFETY PRECAUTIONS listed should be followed to assure safe operation. Cell material should be compatible with the test sample. Cell bodies that show signs of stress cracking, severe pitting, or have damaged set screw holes must not be used. Cell caps showing evidence of the set screw seat being pulled or deformed must not be used. Damaged or Hardware Store set screws must not be used. 1. Loosen the six socket head set screws and remove the cell end cap by pulling it straight out of the cell, using the valve stem as a handle. 2. Check O rings on the valve stems, cell body and cap. Replace any damaged or brittle O rings. Replacement of O rings is normally required after test run above a temperature of 350 F. 3. Repeat 1 and 2 above for the other end cap. 4. Reassemble the end cap and valve stem which is going to be the non-filter end. (The filter end is the end with two little holes in the jacket.) Make sure the six socket set screws are securely tightened and the valve stem is tight. 5. Carefully fill the cell with sample to be tested. Allow to from the top for expansion when the sample is to be heated. 6. Position the filter on the O ring in the cell body. Place the screen on the filter paper, course side up. 7. Install the end cap making sure the set screw seats in the cap are aligned with the set screws in the body. Tighten set screws firmly, then install and tighten the valve stem. 8. Invert and lower the filtration cell assembly into the heating jacket (filter end down) and rotate so that the pin is in the bottom of the cell. This prevents the cell rotating when the

39

valve stems are opened or closed.

C. Pressurizing the Filtration Cell

1. Attach the high pressure hose connected to the 1500 psi gauge side of the manifold, to the top, or inlet, valve stem and insert the locking pin. 2. Close the bleeder valve on the valve stem adapter manifold. 3. Check the T screws on the pressure regulators to be sure that they are unscrewed (counterclockwise) and no pressure will be applied. 4. Open the valve on the Nitrogen bottle slowly and carefully. The bottle pressure will be registered on the middle manifold gauge. 5. Turn the T screw on the left hand regulator clockwise until the desired cell pressure is registered on the gauge.
D. Conducting the Filtration Test

1. Place a graduated cylinder under the cell lower valve stem. 2. Check the temperature of the cell by placing the metal stem dial thermometer in the thermometer well of the cell. As soon as the desired temperature is reached, the test may be started. 3. With an adjustable wrench, open the inlet valve stem turn. If the pressure on the cell pressure gauge of nitrogen manifold has changed from the desired setting, readjust the regulator. If the adjustment is to lower the pressure, momentarily open the bleed valve to reduce the pressure. 4. Set a timer for 30 minutes or other desired filtration test time. 5. With an adjustable wrench, open the lower valve stem on the bottom of the filtration cell turn. This is the start of the test.
E. Test Conclusion and Disassembly

1. Disconnect the filter press-heating jacket from the power source. 2. Close the filtration cell (upper) valve stem. 3. Release the T screws (turn counterclockwise) of the test filtration. 4. Open the bleed valve on the test cell manifold to de-pressurize the system. 5. Remove the upper valve stem locking pin and remove the adapter manifold from the top valve stem. 6. The pressurized cell assembly may be left in the heating jacket or it may be removed to another location for air cooling, or it can be removed from the heating jacket and rapidly

40

cooled with running water. 7. After the cell and the sample in the cell are cool, the cell may be opened. Make sure the open end of the valve stem is pointed away. Then, using the adjustable wrench, open the top valve stem (the one on the opposite end of the cell from the filter) about turn and allow the pressure to bleed off. Make sure all pressure has bled off.

**WARNING**
Do not attempt to remove the cell cap if any pressure remains in the cell. Removing the cell cap while the cell is pressurized could result in serious injury.

8. Once sure that all the pressure has been release, loosen the six socket set screws in the end cap and using the valve stem as a handle, pull the end cap out of the cell. 9. The sample may now be emptied and examined as desired.
Results:

1) Tabulate the following properties: a) Corrected 30-min. fluid loss (ml) b) Filter cake thickness. 2) Graph the following properties vs. temperature: a) Corrected 30-min. fluid loss (ml) 3) Summarize the effects of increasing temperature on the mud and compare the results of each mud system.

41

FIELD TESTING OF CEMENTS Laboratory Experiment No. 5 Regular Cement, Cement Extenders and Cement Weighting Materials
Object:

Investigate the effects of cement extenders and weighting materials on regular neat cement.
Theory:

Lightweight cement slurries are used to reduce hydrostatic pressure on weak formations and to lower slurry cost. Basically, lightweight slurries are made by adding more water to lighten the mixture and then adding cement extenders, such as bentonite clay, which keep the solids from separating. Bentonite is compatible with all additives and may be used to formulate specific cement systems. High-density slurries are used to cement high-pressure wells where increased hydrostatic head is required to prevent formation gas, oil, or water from entering the borehole during cementing operations. Barite (s.g. = 4.23) is a commonly used weighting material and can be used to increase cement slurry density up to 18.0 ppg.
Procedure:

Each group will prepare two 500 ml samples of their three cements at the beginning of lab. Prepare each 500 ml sample in the following manner:
Group 1 Cement 1: Regular cement (32.0 % water). Add 640.0 gr. of cement to 296.0 cc of water already in blender and mix at high speed for 35 seconds. Cement 2: Regular (35.0 % water). Add 583.2 gr. of cement to 315.0 cc of water already in blender and mix at high speed for 35 seconds. Cement 3: Regular cement (40.0 % water). Add 507.4 gr. of cement to 339.0 cc of water already in blender and mix at high speed for 35 seconds. Group 2 Cement 1: Regular cement with 4.0 % bentonite (40.0 % water). Dry mix 19.5 gr. of bentonite with 487.1 gr. of cement and mix with 338.0 cc of water already in blender at high speed for 35 seconds. Cement 2: Regular cement with 8.0 % bentonite (46.0 % water). Dry mix 31.5 gr. of bentonite with 393.2 gr. of cement and mix with 363.0 cc of water already in blender at high

42

speed for 35 seconds. Cement 3: Regular cement with 12.0 % bentonite (51.0 % water). Dry mix 39.6 gr. of bentonite with 329.7 gr. of cement and mix with 380 cc of water already in blender at high speed for 35 seconds.
Group 3 Cement 1: Regular cement with 5.0 % barite (31.0 % water). Dry mix 31.1 gr. of barite with 621.7 gr. of cement and mix with 295.0 cc of water already in blender at high speed for 35 seconds. Cement 2: Regular cement with 15.0 % barite (30.0 % water). Dry mix 88.2 gr. of barite with 588.3 gr. of cement and mix with 292.0 cc of water already in blender at high speed for 35 seconds. Cement 3: Regular cement with 50.0 % barite (28.0 % water). Dry mix 247.5 gr. of barite with 495.1 gr. of cement and mix with 284.0 cc of water already in blender at high speed for 35 seconds.

Each group will test their 3 cements for the following properties: 1. 2. 3. 4. Density (Mud Balance). Plastic viscosity, yield point (Baroid Rheometer). Fluid loss (Filter Press). Compressive strength (Versa Tester).
Note the following:

1. 2. 3. 4.

Perform the fluid loss test LAST. Do a 10-min filtration test and report the corrected 30-min loss. Do the compressive strength determination on 3 molds after waiting 24 hours. Include Cement 1/Group 1 as the 0.0 % additive point in all the tabulations and graphs.

Results:

1) Tabulate the following mud properties: a) Cement density (ppg). b) Plastic viscosity (cp) c) Yield point (lbs/100 sq. ft.). d) Dehydration time (min). e) Corrected 30-min fluid loss (ml). f) Compressive strength (psi). 2) Plot the following cement properties vs. (1) % of water (Group 1), (2) % of bentonite (Group 2), and (3) % barite (Group 3) in the slurry: a) Cement density (ppg) b) Plastic viscosity (cp) 43

c) Yield point (lbs/l00 sq. ft.). d) Corrected 30-min fluid loss (ml). e) Compressive strength (psi). 3) Summarize the results of doing the following experiments: a) Increasing the water concentration of regular cement (Group 1). b) Increasing the bentonite concentration of regular cement (Group 2). [Note: Water content increases according to API minimum requirements.] c) Increasing the barite concentration of regular cement (Group 3). [Note: Water content increases according to API minimum requirements.] 4) Compare the results of using water without bentonite and water with bentonite to extend the cement.

44

FIELD TESTING OF CEMENTS Laboratory Experiment No. 6 Cement Accelerators and Retarders
Object:

Investigate the effects of cement accelerators and retarders on neat cement.

Theory:

Most operations wait for cement to reach a minimum strength of 500-psi before resuming operations. At temperatures below 100 F, common cement may require a day or two to develop 500-psi compressive strength. Low concentrations of cement accelerators (2-4 % by weight of cement) are used to shorten the setting time of cement and promote rapid strength development, thus reducing waiting-oncement (WOC) time. Calcium chloride and sodium chloride are the most common accelerators. With its accelerated thickening time and compressive strength development, calcium chloride is used in whipstock plugs, lost-circulation plugs, and squeeze slurries. Increased well depths and formation temperatures require the use of cement retarders to extend the pumpability of cements. Besides retardation, most retarders affect cement viscosity to some extent. Lignosulfonates and celluloses (which we will discuss in our next experiment) are mild dispersant. Calcium lignosulfonates, derived from wood-pulping processes, are the most common retarders. They are available as either a brown powder or liquid. Their effectiveness is limited to temperatures less than 100 F.
Procedure:

Each group will prepare two samples of their three cements at the beginning of lab. Each sample will be slightly greater than 500 ml. Prepare each 500 ml sample in the following manner.
Group 1 Cement 1: Regular cement with 1.0 % calcium chloride (CaCl) (28.0 % water). Dissolve 7.0 gr. of calcium chloride in 280.0 cc of water already in blender. Add 700.0 gr. of cement and mix at high speed for 35 seconds. Cement 2: Regular cement with 2.5 % calcium chloride (28.0 % water). Similar to Cement 1 but using 17.5 gr. of calcium chloride.

45

Cement 3: Regular cement with 4.0 % calcium chloride (28.0 % water). Same as Cement 1 except use 28.0 gr. of calcium chloride. Group 2 Cement 1: Regular cement with 1.0 % sodium chloride (NaCl) (28.0 % water). Dissolve 7.0 gr. of sodium chloride in 280.0 cc of water already in blender. Add 700.0 gr. of cement and mix at high speed for 35 seconds. Cement 2: Regular cement with 2.5 % sodium chloride (28.0 % water). Same as Cement 1 except use 17.5 gr. of sodium chloride. Cement 3: Regular cement with 4.0 % sodium chloride (28.0 % water). Same as Cement 1 except use 28.0 gr. of sodium chloride. Group 3 Cement 1: Regular cement with 0.1 % Lignin HR4 retarder (28.0 % water). Dissolve 1.4 gr. of retarder in 280.0 cc of water already in blender. Add 700.0 gr. of cement and mix at high speed for 35 seconds. Cement 2: Regular cement with 0.25 % Lignin HR4 retarder (28.0 % water). Same as Cement 1 except use 1.75 gr. retarder. Cement 3: Regular cement with 0.5 % Lignin HR4 retarder (28.0 % water). Same as Cement 1 except use 3.5 gr. retarder.

Each group will test their 3 cements for the following properties: 1. Density (Mud Balance). 2. Fluid loss (Filter Press). 3. Compressive strength (Versa Tester).
Note the following:

1. 2. 3. 4.

Perform the fluid loss test LAST. Do a 10-min filtration test and report the corrected 30-min loss. Do the compressive strength determination on 3 molds after waiting 24 hours. Include Cement 1/Group 1 from Laboratory Experiment No. 4 as the 0.0 % additive point in all the tabulations and graphs.

Results:

1) Tabulate the following mud properties: a) Cement density (ppg). b) Plastic viscosity (cp) c) Yield point (lbs/100 sq. ft.). 46

d) Dehydration time (min). e) Corrected 30-min fluid loss (ml). f) Compressive strength (psi). 2) Plot the following cement properties vs. (1) % of calcium chloride (Group 1), (2) % of sodium chloride (Group 2), and (3) % Lignin HR4 retarder (Group 3) in the slurry: a) Cement density (ppg) b) Plastic viscosity (cp) c) Yield point (lbs/l00 sq. ft.). d) Corrected 30-min fluid loss (ml). e) Compressive strength (psi). 3) Summarize the results of doing the following experiments: a) Increasing the calcium chloride content of regular cement (Group 1). b) Increasing the sodium chloride content of regular cement (Group 2). c) Increasing the Lignin HR4 Retarder content of regular cement (Group 3). 4) Compare the results of using calcium chloride as cement accelerators.

47

FIELD TESTING OF CEMENTS Laboratory Experiment No. 7 Water Loss Additives and Dispersants
Object:

Investigate the effects of water loss additives and dispersants on neat cement.
Theory:

Fluid-loss additives improve primary cement jobs because they have the ability to: 1. Prevent cement degradation in the annulus. This helps prevent stuck pipe, helps prevent loss of returns, and helps to bring cement to the desired height. 2. Prevent gas migration. The viscosity and gelation properties of slurries containing fluidloss additives help solve this problem. 3. Improve bonding. The bonding qualities of cements containing fluid-loss additives are also very good. 4. Minimize formation damage. By reducing the amount of filtration lost into sensitive formations, fluid-loss additives help insure better formation productivity. Fluid-loss additives are polymers. The most common are cellulose derivatives and they are also used to control the rate of dehydration when squeezing. This is especially true when squeezing perforations. Dispersants reduce slurry viscosity, allow slurry turbulence at lower pump rates, allow heavier slurries with less water and less weighting materials, and help provide fluid-loss control for densified slurries. The most common dispersants are aryl sulfonates used in concentrations of 0.3 % to 2.0 % by weight of cement. Neat cement slurries with densities above 17 ppg are difficult to mix. By using a high molecular weight polymer, however, slurries may be densified to 18 ppg without using a weighting material. For slurries heavier than 18 ppg a combination of dispersant and weighting agent is used.
Procedure:

Each group will prepare two of their three cements at the beginning of lab. Prepare each 500 ml sample in the following manner:
Group 1 Cement 1: Regular cement with 0.5 % aryl alkyl sulfonate (CFR-2) (28.0 % water). Dry mix 3.5 gr. of CFR-2 with 700.0 gr. of cement and mix with 280.0 cc of water already in

48

blender at high speed for 35 seconds. Cement 2: Regular cement with 1.0 % aryl alkyl sulfonate (CFR-2) (28.0 % water). Same as Cement 1 except use 7.0 gr. of CFR-2. Cement 3: Regular cement with 2.0 % aryl alkyl sulfonate (CFR-2) (28.0 % water). Same as Cement 1 except use 14.0 gr. of CFR-2.
Group 2 Cement 1: Regular cement with 2.0 % organic polymer (28.0 % water). Mix 14.0 cc of organic polymer with 280.0 cc of water already in blender. Add 700.0 gr. of cement and mix at high speed for 35 seconds. Cement 2: Regular cement with 6 % organic polymer (28.0 % water). Same as Cement 1 except use 42.0 cc of organic polymer. Cement 3: Regular cement with 10% organic polymer (28% water). Same as Cement 1 except use 70.0 cc of organic polymer. Group 3 Cement 1: Regular cement with 0.1 % cellulose (Flocelle) (28.0 % water). Dry mix 0.1 gr. of Flocelle with 700.0 gr. of cement and mix with 280.0 cc of water already in blender at high speed for 35 seconds. Cement 2: Regular cement with 1.0 % cellulose (28.0 % water). Same as Cement 1 except use 7.0 gr. of Flocelle. Cement 3: Regular cement with 2.0% cellulose (28.0 % water).Same as Cement 1 except use 14.0gr. of Flocelle.

Each group will test their cements for the following properties: 1. 2. 3. 4. Density (Mud Balance). Plastic viscosity, yield point (Baroid Rheometer) Fluid loss (Filter Press). Compressive strength (Versa Tester).

Note the following:

1. 2. 3. 4.

Perform the fluid loss test LAST. Do a 10-min filtration test and report the corrected 30-min loss. Do the compressive strength determination on 3 molds after waiting 24 hours. Include Cement 1/Group 1 from Laboratory Experiment No. 4 as the 0.0 % additive point in all the tabulations and graphs.

49

Results:

1) Tabulate the following mud properties: a) Cement density (ppg). b) Plastic viscosity (cp) c) Yield point (lbs/100 sq. ft.). d) Dehydration time (min). e) Corrected 30-min fluid loss (ml). f) Compressive strength (psi). 2) Plot the following cement properties vs. (1) % of CFR-2, (2) % of organic polymer, and (3) % of Flocelle in the slurry: a) Cement density (ppg) b) Plastic viscosity (cp) c) Yield point (lbs/l00 sq. ft.). d) Corrected 30-min fluid loss (ml). e) Compressive strength (psi). 3) Summarize the results of doing the following experiments: a) Increasing the aryl alkyl sulfonate content of regular cement (Group 1). b) Increasing the organic polymer content of regular cement (Group 2). c) Increasing the cellulose content of regular cement (Group 3). 4) Compare the results of using organic polymer and Flocelle as water loss control additives.

50

SURFACE BOPSTACK WELL CONTROL Laboratory Exercise No. 8 Simulator Orientation

Object:

Become acquainted with the components of the CS Inc. DS-20FS/W/P rig floor simulator.
Theory:

The results of a hydrocarbon well blowout can be disastrous. Natural gas or crude flowing uncontrollably at the surface can take human life, destroy millions of dollars worth of equipment, and cause irreparable damage to the environment. Drilling rig personnel must be properly trained to prevent the occurrence of blowouts. Rig floor simulators allow rig personnel to practice well control procedures, to test the principles and theory underlying these procedures, and to become familiar with the equipment used during well control operations. Before the simulator can be effectively utilized, however, the student must have an understanding of its components and operation.
Procedure:

The lab instructor will conduct a tour of Penn States rig floor simulator, a DS-20FS/W/P. The following topics will be covered. 1. Rig components used during normal drilling operations. 2. Rig components used during well control operations. 3. Simulator representations of actual rig components. 4. Simulator components used to program and control simulator operations.
IMPORTANT:

1. The DS-20FS/W/P is a sensitive piece of machinery. 2. Special care must be taken not to damage simulator components. 3. DO NOT touch any control on the instructors program panel. 4. DO NOT lean against or stand on any simulator component. 5. DO NOT set textbook, notebooks, or coats on any simulator component. 6. DO NOT force open any valves if they appear to be stuck.

51

7. DO NOT excessively tighten any valves to close them. 8. DO NOT raise the Kelly bushing more than halfway to the ceiling. 9. The general rule to use is WHEN IN DOUBT ASK THE LAB INSTRUCTOR BEFORE PROCEEDING.
Results:

1) Reproduce the list of DOs and DONTs for proper simulator operation that the lab instructor covers at the beginning of lab. The list will be posted and reviewed by the lab instructor at the beginning of each lab meeting and WILL BE STRICTLY ENFORCED! 2) Make a line drawing of each of the simulator components listed below showing the position of each gauge or control found on the component. Use a different piece of paper for each component and make the drawings large enough so that space is available to label each gauge and control. Include a sentence or two for each label that describes the function of that particular part. i) ii) iii) iv) v) vi) vii) viii) ix) Drawworks console. Drillers console. Brake handle and foot throttle. Surface BOP stack control panel. Remote choke panel. Remote mud box. Drill pipe visual display. Choke manifold. Standpipe manifold.

3) Draw a schematic of the drilling mud circulation system on the simulator. Show the path followed by the mud during normal drilling operations. Show the path followed by the mud during well control operations.

52

SURFACE BOP STAC WELL CONTROL Laboratory Exercise No. 9 Simulator Operation
Object:

Practice working the controls of the CS Inc. DS-20FS/W/P rig floor simulator to observe the effects of different mud densities on the rate of penetration (ROP).
Theory:

The rate at which the drill bit can penetrate the formation rock is an important economic consideration during drilling operations. An optimal penetration rate reduces the amount of time the rig spends on location and thus minimizes the cost of leasing the rig. The ROP is a function of many factors including bit type, weight-on-bit (WOB), bit RPM, rock strength, differential pressure, etc. Differential pressure refers to the difference between the pressure exerted by the drilling mud at total depth and the formation pressure at that depth. Differential pressure is a function of mud density because muds having different densities will exert different pressures at the same depth. A correlation between mud density and ROP can be obtained by changing mud weights and measuring the ROP while through the same formation.
Procedure:

The lab instructor will first review the rules that must be followed whenever operating the simulator. At the start of the exercise the bit should be hanging slightly above bottom and rotating slowly. In addition, the mud pump should be turned on so that the drilling mud is slowly circulating. All well parameters such as total depth, hoe size, drill pip capacity, etc., and all drilling parameters such as WOB, rotary speed, pump speed, etc., will be given to you by the lab instructor at this time. Initial mud weight will be 19.0 ppg. One student will be designated the driller and it will be the drillers responsibility to run the bit to bottom and to drill ahead while making sure the that the specified drilling parameters are held as constant as possible. The driller should follow the procedure given below: 1. With the bit still hanging off bottom, bring the mud pump up to the proper strokes per minute (SPM). 2. Remove tie-down chain from the brake handle and lift up on the brake handle until the drill pipe begins to slowly fall into the hole.

53

3. Make sure the bit is still rotating slowly and watch the WOB indicator. When the bit touches bottom the WOB indicator will show the bit taking on weight. Slowly increase the WOB to the proper value while steadily increasing bit RPM. 4. Stop the drill pipe from falling when the proper WOB is reached by pushing down on the brake handle. Double check mud pump SPM and bit RPM to make sure they are at the proper values. 5. Wait for the geolograph to make a tick mark. Another tick mark will be made when 1 foot of hole has been drilled. The time between tick marks should be measured and the ROP (ft/hr) calculated. Also, record the drill pipe pressure. 6. After 1 foot of hole has been drilled in this manner the bit should be returned to its original position. Decrease the bit RPM to zero. Lift up on the brake handle and step on the foot throttle. Raise the bit until the WOB falls to zero. Adjust the bit RPM and the mud pump SPM to their standby levels. Another student will now be designated the driller and follow the same procedure for a mud weight of 17.0 ppg. Continue in this manner, decreasing the mud weight in increments of 2.0 ppg, until all of the students have had a turn at the controls.
Results:

1) Plot ROP (ft/hr) vs. mud density (ppg). 2) Plot ROP (ft/hr) vs. differential pressure (psi). 3) Summarize the effects of decreasing mud density on ROP.

54

SURFACE BOP STAC WELL CONTROL Laboratory Exercise No. 10 The Soft Shut-In Procedure
Object:

Practice detecting gas kicks and shutting in the well using the soft shut - in procedure.
Theory:

When the bit passes through an impermeable cap rock into a porous and permeable formation a drilling break can occur. A drilling break is simply a sudden, sharp increase in the penetration rate. It indicates that you are in a situation in which a blowout could occur because a porous and permeable formation could contain abnormally pressured gas. It does not indicate that a kick is occurring. It is merely a warning signal that tells you to proceed with caution. Two other indicators, however, will tell you that a kick is definitely occurring. The primary indicator is a flow rate increase in the mud return line. A flow rate increase will always occur before the secondary indicator, an increase in the mud pit volume is noticeable. The flow rate meter and mud pit gain/loss indicator monitor the values of these two positive kick indicators, respectively. A flow check should be performed as follows if there is ever a doubt about whether or not the well is kicking: 1. Stop rotating and pull the bit off bottom. 2. Shut off the mud pumps. 3. Check for flow. A kick is definitely occurring if the well continues to flow after the mud pump has been shut off and the well should be immediately shut in. Shutting the well in stops the influx of abnormally pressured gas into the wellbore because the abnormal formation pressure is balanced by the increase in shut-in drill pipe and shut-in casing pressure. The well should be shut in using the soft shut-in procedure. This procedure allows the pressure in the wellbore to build up slowly and minimizes the possibility of pressure surges that could damage the casing and surface equipment or fracture the formation.
Procedure:

The lab instructor will first review the rules that must be followed whenever operating the simulator. At the start of the exercise the bit should be hanging slightly above bottom and rotating 55

slowly. In addition, the mud pump should be turned on so that the drilling mud is slowly circulating. All well parameters and drilling parameters will be given to you by the lab instructor at this time. One student will be designated the driller, one will be designated the choke operator, and one will be designated the BOP operator. After the flow rate and mud pit volume increase, alarms are set in a manner described by the lab instructor, the driller will begin to drill ahead and should watch closely for the occurrence of any kick indicators. Once the driller decides that a kick is occurring the well should be shut in following the soft shut-in procedure: 1. The driller stops rotation, picks up the drill pipe until the WOB falls to zero, and continues to pick up the drill pipe until the Kelly bushing is 3 - 4 above the rotary table. 2. The driller shuts off the mud pumps. 3. The BOP operator (1) opens the choke line valve on the BOP stack, and (2) closes the annular preventer. Both pieces of equipment are operated by first depressing the master air valve shut-off switch and then moving the equipment control switch to the open or closed position. Both switches should be engaged until the red light goes off or comes on to signal that equipment is open or closed, respectively. 4. The choke operator closes the remote choke. 5. Let the pressures stabilize and read the shut-in drill pipe and shut-in casing pressures. This procedure should be repeated until everyone has had a chance to be the driller, choke operator, and BOP operator.
Results:

1) Describe the 3 kick indicators used in this exercise. 2) Describe the flow check procedure. 3) Describe the soft shut-in procedure.

56

SURFACE BOP STAC WELL CONTROL Laboratory Exercise No. 11 The Wait and Weight Method
Object:

Practice killing a well using the wait and weight method of well control.
Theory:

Most methods of well control have at least three characteristics in common: (1) the gas kick is circulated out to the hole, (2) additional formation gas is prevented from entering the wellbore, and (3) the drilling mud density is increased so that the hydrostatic pressure exerted by the mud column will counterbalance the abnormal formation pressure. Once the proper kill weight mud has been completely circulated through the system the well is said to be killed or dead and normal drilling operations can be resumed (with caution!). One of the most important aspects of well control is to prevent the influx of additional gas into the wellbore. This is accomplished by keeping the pressure exerted by the mud column in the drill pipe at the bottom of the hole constant while the gas kick is being circulated to the surface. Shutting in the well temporarily stops more gas from flowing into the wellbore because the abnormal formation pressure is balanced by the mud hydrostatic pressure plus the shut-in drill pipe pressure. In fact, the value of the shut-in drill pipe pressure is exactly equal to the pressure differential between the abnormal formation pressure and the mud hydrostatic pressure. During the wait and weight, while the kick is being circulated to the surface the choke is adjusted so that the circulating bottom hole pressure balances the abnormal formation pressure. The circulating bottom hole pressure can be calculated by adding the hydrostatic pressure of the mud in the drill string to the circulating drill pipe pressure. Several terms should be defined at this point: 1. Kill rate pressure or slow circulating rate pressure - This is the drill pipe pressure required to circulate original weight mud through the wellbore at a reduced pump speed called the kill rate. The kill rate pressure must be measured before the well kicks. 2. Shut-in drill pipe pressure - This is the extra pressure required to control the kicking formation. 3. Initial circulation pressure - This is the value that the circulating drill pipe pressure should have at the start of the wait and weight procedure. It is equal to the kill rate pressure plus the shut-in drill pipe pressure.

57

The object of the wait and weight method is to circulate kill weight mud into the well through the drill pipe, to circulate the gas kick out of the hole through the annulus, and to keep the abnormal formation pressure balanced by the mud column pressure in the drill pipe all at the same time. As soon as the mud pits are filled with kill weight mud the choke is opened and the mud pump is brought up to the kill rate. The choke is quickly adjusted so that the drill pipe pressure gauge reads a value equal to the initial circulating pressure. As more kill weight mud is circulated down through the drill pipe the pressure exerted by the column of mud in the drill pipe is increased because the lighter original mud is displaced by the high density kill mud. The circulating drill pipe pressure must be reduced accordingly or else the increased bottom hole pressure could become great enough to fracture the formation when the kill weight mud finally reaches the bottom of the hole and begins to displace original mud out of the annulus. When the kill mud reaches the bit the drill pipe pressure is reduced to a value called the final circulating pressure. Drill pipe pressure is held constant at the final circulating pressure during the remainder of the kill procedure because there is now only one type of mud in the drill string and the hydrostatic pressure there is constant. The well should be dead when kill weight mud reaches the surface through the annulus.
Procedure:

The lab instructor will first review the rules that must be followed whenever operating the simulator. At the start of the exercise the bit should be hanging slightly off bottom and slowly rotating. In addition, the mud pump should be turned on so that the mud is slowly circulating. All well parameters and all drilling parameters will be given to you by the lab instructor at this time. Everyone should fill in the prerecorded information portion of the wait and weight kill sheet. One student will then be designated the driller, one the choke operator, and one the BOP operator. First, the kill rate pressure should be measured. Bring the mud pump SPM up to the first kill rate record that kill rate pressure. Then, adjust the pump SPM to the second kill rate pressure and record that kill rate pressure. Follow the same procedure to measure and record the two kill rate pressures for the second mud pump. The driller should then start to drill ahead and watch for kick indicators. As soon as the kick is detected, the well should be shut in following the soft shut-in procedure. Read and record the shut-in drill pipe pressure and shut-in casing pressure after they have stabilized. Record the pit volume increase. Follow the directions on the kill sheet increase, final circulating pressure, surface-to-bit strokes, and bit-to-surface strokes. 58

Fill in the circulating drill pipe pressure schedule at the bottom of the kill sheet. Dial up the the proper kill weight mud on the remote mud box. You are now ready to kill the well by the wait and weight method. The Wait and Weight method is outlined below: 1. Starting with the well completely shut-in, the choke operator will first crack open the choke and then the driller will slowly but steadily bring the mud pump up to the kill rate. The choke operator should keep the casing pressure constant by opening or closing the choke as the pump is brought up to speed. 2. As soon as the mud pump is at the kill rate the choke operator should adjust the choke so that the drill pipe pressure equals the initial circulating pressure. 3. The driller will continue to pump kill mud into the hole at the kill rate. At the same time the choke operator will reduce the drill pipe pressure from the initial circulating pressure to the final circulating pressure according to the pressure reduction scheduled at the bottom of the well control worksheet. 4. The choke operator will maintain the final circulating pressure after the kill weight mud reaches the bit until the kill weight mud appears at the surface. 5. When the kill mud reaches the surface the crew should do a soft shut-in and check the shut-in drill pipe and casing pressures. The well is assumed to be dead only if both pressures are zero. As many people as possible should have a chance to operate the choke during this exercise. The entire exercise should be repeated with different people at the various stations if time allows.
Results:

1) Describe the wait and weight method of well control. 2) Complete the wait and weight worksheet for your well control problem. 3) List the advantages and disadvantages of the wait and weight method.

59

CEMENT HEAD LABORATORY Laboratory Exercise No. 12 Cement a Casing String

Object:

Evaluate the techniques of cementing casing in a well.

Theory:

Different cementing equipment and placement techniques are used for cementing casing strings, cementing liner strings, setting cement plugs, and squeeze cementing. A casing string is different from a liner string in the fact that the casing extends to the surface, while the liner is attached to the subsurface casing previously cemented in the hole. Cement plugs are placed in open hole or in casing before abandoning a lower portion of the well. Cement is squeezed into lost-circulation zones, abandoned casing perforation, or a leaking cemented zone to stop undesired fluid movement.
Cementing Casing

When the casing string is ready to be cemented the cement slurry is prepared in a special cementing unit for the type of the job (truck mounted for land jobs, skid mounted for offshore). The cement slurry is pumped from the unit to a special cementing head screwed into the top joint of casing. When cementing begins, the bottom rubber wiper plug is released from the plug container ahead of the cement slurry. The plug wipes the mud from the casing ahead of the slurry to minimize contamination of the cement with the mud. The plug reaches the float collar and stops. Continuing to pump cement causes a diaphragm in the plug to rupture (a spike will occur in the pump pressure). This allows the cement slurry to be displaced through the plug and into the annulus. After the desired volume of cement slurry is pumped into the casing, the top wiper plug is released from the plug container. The top plug displaces the cement plug by pumping drilling mud into the casing behind the top plug. When the top plug reaches the bottom plug a pressure increase will be encountered which signifies the end of the displacement operation.
Procedure:

1. The lab instructor will provide everyone with the depth, hole diameter, and casing size. 2. The volume of the annulus must be calculated using this data (use a safety factor of 1.2). 3. This will be the volume of cement slurry that is needed to be pumped. 4. The number of strokes required to pump this volume must then be calculated.

60

At the start of the exercise the mud pumps will be on so that the mud is slowly circulating. Stop circulation and pick up off the bottom. Assume that the casing string is now at the correct depth to be cemented. Unhook the Kelly and hook up to the cement head. Load the bottom plug into the cement head and then load the top plug. Open the cement head valve to allow flow of the cement slurry and turn on the cement pumps. Remove the pin supporting the top plug to allow it to lead the slurry to the float collar. When a spike is seen in the pump pressure the plug has reached the float collar. Pump until the total number of strokes needed for the desired cement volume is obtained. At this time release the top plug, discontinue pumping cement and resume pumping mud until the top plug reaches the bottom plug. Look for a spike in the pump pressure and shut the mud pumps down.
Results:

1) Describe the method of cementing the casing. 2) Compare the method completed in the lab with other methods used in the industry. 3) Describe other uses of cementing.

61

APPENDIX A

MUD ADDITIVES

62

MUD ADDITIVES1
Mud control can be divided into three basic categories: the control of mud weight, the control of viscosity and gel strength, and the control of water loss. Various mud additives have been developed for each of these areas of control.
Control of Mud Weight

Mud weight control is almost synonymous with the control of solids. The mud weight requirements should be based on that weight required to control formation pressures. For under-pressured reservoirs (i.e. formations with pore pressures less than 0.433 psi/foot depth) mud weight can be reduced to levels below the fresh water gradient by using oil, oil and fresh water, or by aerating the fluid column. The use of air (or natural gas) alone as a drilling fluid is also an acceptable practice, although this technique is restricted to areas where there are no high volume water sands to be penetrated. Weighted muds are defined as those where barite or some other high density solid has been added to increase mud weight.

Control of Viscosity and Gel Strength

The control of viscosity or mud thickness will of course depend on the operators objectives. Viscosity may be maintained at high levels to ensure adequate hole cleaning. Additives, such as some of the polymers, may be added to increase the mud thickness for adequate hole cleaning while keeping the mud weight and total solids content at low levels. With weighted muds some operators have used polymers for increasing thickness in order to keep clay solids that provide support for the barite, to a minimum. In general, if there are no specific hole requirements, the operator prefers to use the thinnest possible drilling fluid. Thinning is also emphasized when using weighted muds close to the fracture gradient of exposed formations. When more viscosity is desired it may be obtained by (1) adding Bentonite, (2) flocculating the clay solids, and (3) adding polymers designed for the purpose. Bentonite is the primary viscosity builder in the mud system. If fresh water is being used Bentonite will increase viscosity rapidly with only small increases in mud weight. Flocculation of the clays in a fresh water mud is also a quick and cheap method of increasing viscosity. The flocculation can usually be done by adding lime or cement. Another method for thickening mud is the use of specific polymers.

Moore, Preston L., Drilling Practices Manual, The Petroleum Publishing Co.

63

There are several different polymers available. Basically, they can be divided into three groups; (1) the polymers that thicken the mud by acting on the clay solids, (2) polymers that are colloidal in nature and essentially provide a substitute for bentonite, and (3) the polymers that thicken the liquid phase and do not react with bentonite. Viscosity control is generally in terms of reducing mud thickness. Methods used for control include mechanical aids, water dilution and chemical thinners. The most widely used of these methods is the chemical thinners. Table 1 includes some of the more common mud thinners.

Table 1. Drilling mud thinners

Chemical Sodium acid pyro Phosphate Sodium tetraphosphate Chrome Lignosulfonate Liginite Tannin Surfactants pH of 1% solution 4.3 8.0 7.0 3.2 5.0 Limitations Decomposed and forms flocculating agent above 175 F. Not effective in the presence of large quantities of calcium Same as 1.0 Material starts to decompose at temperatures above 300 F. pH needs to be at least 9.0. Material starts to decompose at temperatures above 350 F. pH needs to be at least 9.0. Not very effective if pH of mud is less than 11.0. Many types, temperature stability above 300 F may be a problem. Most are more expensive than other materials

Control of Water Loss (Filtration Control)

The filtration rate is generally controlled for the following two reasons: (1) to control the thickness and characteristics of the filter cake which is deposited on permeable formations and (2) to limit the total filtrate that enters underground formations. Filter cake thickness and the friction between the filter cake and the drill string relate to the problems of (1) differential pressure sticking, (2) torque and drag while drilling and tripping the drill string, (3) running of wireline tools and casing strings and (4) sidewall coring. An increase in filter cake thickness increases the area of contact between the drill string and the filter cake and for a given friction coefficient increases the danger of sticking the drill string and also increases the torque and drag on the drill string. The running of wireline tools and casing is restricted by the reduction in hole size as the filter cake gets thicker. A thick filter cake may prevent any formation recovery on a wireline test. For these problems the operator is not concerned with the actual loss of filtrate. The filtrate loss is used to indicate the potential thickness of the filter cake. The problems of differential pressure sticking and torque and drag are related primarily to high weight drilling muds in deep high temperature environments.

64

Operators are concerned with the total filtrate entering underground formations for the following reasons: (1) some believe that shale sloughing is caused by filtrate invasion into the shales, (2) they believe results of formation evaluation methods may be affected by filtrate invasion, and (3) they believe formation productivity is often affected by filtrate invasion, especially in low permeability sands. Additives of common usages to control filtration are shown in Table 2.
Table 2. Additives for the control of filtration rate
Provides a better basic filter cake Reduces filtration by deflocculating the mud also increases the viscosity of Metal lignosulfonates the filtrate. Starts braking down at 300 F. Not very effective above 350 F. Reduces filtration rate by deflocculating and plugging open spaces in filter Lignite cake. Starts breaking down at 300 F. Effective to reduced degrees above 400 F. Sodium Carboxymethylcellulose, Reduces filtration rate by coating solids and sometimes by minimizing CMC flocculation. Starts breaking down at 300 F. Reduces filtration rate by coating solids. Will spoil in a fresh water environment where pH is less than 11.5. Also a salt concentration of Starch 250,000 ppm will prevent spoiling in any pH water. Breaks down rapidly when temperature exceeds 275 F. Bentonite

Baroid Mud Additives

Baroid Petroleum Services Division N.L. Industries, Inc distributes all the additives used in the mud experiments in the first portion of this lab manual. Brief descriptions of the Baroid mud additives are shown in Table 3.
Table 3. Baroid mud additives
Use General purpose gel-forming Selected, finely colloid used to adjust viscosity, AQUAGEL ground bentonite gel strength, and reduce filtrate clay. loss. Sodium tetra BARAFOS phosphate in dry A polyphosphate mud thinner. granular form. Processed barite Increasing mud density and BAROID (barium making low-solids muds. sulphate). Modified lignite in black, freeflowing power form. Additive Material Features A universally used mud project for both rotary and cable tool drilling. Yields 100 barrels of 15 centipoises drilling mud per ton of AQUAGEL. An effective dispersing agent for clays; has little effect on pH of muds. Recognized as the industrys standard mud weighting material. Low unit cost. High solubility in normal pH muds. Stable at high drilling temperatures. Eliminates or reduces the need for adding raw caustic soda at the rig. Good tolerance for soluble contaminants. Complements other thinners and reduces the need for special filtration control agents.

CC-16

Thinning and filtration control in fresh water muds.

65

Table 3. Baroid mud additives (cont.)

Use Features For making ultra-heavy drilling muds to kill wells of GALENA Makes mud weighing up to 321b/gal. abnormally high pressure. Also used to weight cement slurries. Allows continued use of mud that would Specially otherwise be discarded because of processed, preAn organic colloid for reducing contamination by salts, acids, cement, IMPERMEX gelatinized starch filtrate loss of any drilling mud. gypsum, anhydrite, and other deleterious power. substances. Produces minimum filtration rate in fresh or salt water. An effective means of controlling viscosity and filtration in either fresh water or salt Modified guar To control viscosity and water low-solids mud, while reducing the LOLOSS gum. filtration in low-solids muds. amount of formation solids dispersed in these muds. Particularly effective in brine workover fluids. Ferrochrome A chemical thinner for drilling lignosulfonate, muds, especially for muds Permits use of gyp muds for deep drilling; Q-BROXIN non-caking, light contaminated with salt, allows use of salt water for mud makeup; brown, water gypsum, or both, or as a general emulsifies oil in mud. soluble powder. utility thinner. High yield (200 bbl/ton), Easy and fast to To make high viscosity mud mix. Low cost. Improves wall building. Aids faster than with ordinary clays. QUICKHigh-yield in preventing lost circulation. Does not Used particularly in drilling GEL bentonite. ferment. Reduces water loss. Only half as seismic shot holes and water much needs to be transported compared to wells. other bentonites. Sodium acid As a thinner, dispersant which Used to lower pH of contaminated muds. Is SAPP pyrophosphate. also adds pH control. very sensitive to concentration. As a suspending agent in Dry ground Yields 130 barrels of 15 centipoise mud per ZEOGEL drilling muds of any salt attapulgite clay. ton in saturated salt water. concentration. Additive Material Pulverized lead ore with a specific gravity of about 6.8

66

Table 4. Materials for Drilling Fluid Systems

Maker or Distributor
Magcobar Baroid Div. National Lead Co. Atlas Mud Company Atlas Mud Company Baroid Div. National Lead Co. Magcobar Milwhite Mud Sales Company Baroid Div. National Lead Co. #Cherokee Laboratories *# *# Baroid Div. National Lead Co. Mud Control Laboratories Mud Control Laboratories Mud Control Laboratories Mud Control Laboratories Mud Control Laboratories Baroid Div. National Lead Co. Mud Control Laboratories Mud Control Laboratories #E.I. duPont United Engineering Corp. #American Cyanamid Corp. Milwhite Mud Sales Co. *# #Dow Chemical Co. #Drilling Specialties, Inc. #Northern Chemical Sales Baroid Div. National Lead Co. Magcobar Baroid Div. National Lead Co. Magcobar *# Milwhite Mud Sales Corp. *#
#Several distributing companies

Product Trade Name

Fresh Water Muds Description Product Trade Name Maker or Distributor

Fresh Water Muds (cont.) Description

Alkatan Aquagel Atlas Gel Atlas Lig Barafos Barium Carbonite Barium Carbonite Baroco Benex Bicarb. of Soda Caustic Soda Carbonox Controlgel Caso Control M-D Controltan Controlcal Cellex

Controloid Controlsol C-M-C

Cronox 211

Cypan Caltrol Calcium Chloride Dowcide G Driscose (Sev. Grades)

Magcobar Brown Mud Co. #Westvaco #American Bitumul & Asphalt Baroid Div. National Baroid Div. National #Gibralter Minerals Baroid Div. National Lead Co. Baroid Div. National Lead Co. Baroid Div. National Lead Co. Magcobar #Dril-Kem Marathon Chemical Corp. #Minnesota Mining & Mfg. Milwhite Mud Sales Co. #* #Gibralter Minerals Milwhite Mud Sales Co. Baroid Div. National Lead Co. Alpine Mud Service Macco Corp. Magcobar Magcobar Magcobar May Brothers, Inc. May Brothers, Inc. May Brothers, Inc. May Brothers, Inc. May Brothers, Inc. Macco Corp.

Dakolite Emulsifier SMB Emulsite E P Mudlube Foxit Graphite Green Band Gypsum

Caustic quebracho Wyoming bentonite Wyoming bentonite Lignitic compound Sodium tetraphosphate Barium carbonate Barium carbonate Sub-bentonite Sodium polyacrylate Bicarbonate of soda Sodium hydroxide Organic thinner Bentonite Potassium stearate Drilling detergent Lignite Calcium lignosulfonate Sodium carboxymethylcellulose Pregelatinized starch Nonionic surfactant Sodium carboxymethylcellulose Fresh water corrosion inhibitor Sodium polyacrylate Calcium chloride Calcium chloride Bactericide Sodium carboxymethylcellulose Processed lignite Inorganic emulsifier Caustic lignite Extreme pressure lubricant Polyelectrolyte Graphite lubricant Sub-bentonite Gypsum #Archer-Daniels-Midland Milwhite Mud Sales Co. Milwhite Mud Sales Co. Milwhite Mud Sales Co. Milwhite Mud Sale Co. #Commercial Solvents Corp. Mud Control Laboratories Milwhite Mud Sales Co. Milwhite Mud Sales Co. Magcobar #Pacific Lumber Company

__________________________________________________________________________

*Several packaging companies

High Yield Hydrogel Hexaphos Hydropel Hydrocarb Hydrotan H.Q.M. Starch Impermex Impermex Preservative Kero-X Kwik-Thik Kemical Kembreak Kylo Ligco Lime Lube-Flo Lubri-film Lignox Lig-No-Sol Maccogel Magcogel Magcophos Mc Quebracho May Gel May Clay Maylig Maystarch Maycol Maco-Hex. Maccoflos Macco-Lig Mikol Starch Milgel Mil Graphite Milstarch Mil Flo Mud-Bac Mud Floc Mil-Natan 1-2 Mil Quebracho My-Lo-Jel Palcotan

Sub-bentonite Bentonite Phosphate Emulsified asphalt Caustic carbonox Caustic tannin Grain-based starch Pregelatinized starch Formaldehyde compound Defoaming agent Extra high-yield bentonite Quick lime Calcium lignosulfonate Sodium polyacrylate Mineral lignite Calcium hydroxide Ground gilsonite Extreme Pressure lubricant Calcium lignosulfonate Modified lignosulfates Wyoming bentonite Wyoming bentonite Sodium tetraphosphate Quebracho Wyoming bentonite Sub-bentonite Mineral lignite Pregelatinized starch Calcium chloride Complex phosphates Mineral lignite Pregelatinized starch Wyoming bentonite Graphite Pregelatinized starch Modified polyflavinoid comp. TrisNitro (bactericide) Clocculant Caustic quebracho Quebracho (pure) Pregelatinized starch Lignosulfonate

67

Table 4. Materials for Drilling Fluid Systems (cont.)

Fresh Water Muds (cont.)

Fresh Water Muds (cont.)

Product Trade Name

#Pacific Lumber Company Alamo Lumber Co. Macco Corp. #Los Angeles Chemical #Westvaco *# *# Mud Control Laboratories Baroid Div. National Lead Co. Magcobar Salt Water Muds Ala-Sol Alpine Gel Atlas Salt Gel Atlosol S Attapulgus 150 Ceox Controlfoam Cronox 609 Defoamer No. 23 Emulsifier S F-S Clay Florigel Florigel H-Y Heviwater Maysal Clay Salt Salt Gel Salt-Drill Salt Water Gel Super Sal Attapulgite clay Attapulgite clay Attapulgite clay Anionic-nonionic surfactant Attapulgite clay Emulsifier Defoamer Corrosion inhibitor Mud defoamer Nonionic emulsifier Attapulgite clay Attapulgite clay Attapulgite clay Mud dispersant Attapulgite clay Sodium chloride Attapulgite clay Hemlock bark extract Attapulgite clay Attapulgite clay Air/Gas Drilling Materials Foaming agent #Atlas Chemical Industries Atlas Mud Co. #American Cyanamid Dowell Div., Dow Chemical Antara Chemical Gafen Fa-5 Antara Chemical Polar organic Chemical grout Foaming agent Foaming agent fresh to mod. salt Foaming agent, saturated salt Alamo Lumber Co. Alpine Mud Service Atlas Mud Co. Atlas Chemical Ind. Min. & Chem. Philipp Mud Control Laboratories Mud Control Laboratories United Engineering Corp. Baroid Div. National Lead Co. #Mud Engineering Supplies United Engineering Corp. Floridin Co. Floridin Co. Dowell Div., Dow Chem. May Brothers, Inc. *# Magcobar #Rayonier, Inc. Milwhite Mud Sales Co. Superbar Sales *# #E. I. DuPont Baroid Div. National Lead Co. #Rayonier, Inc. #International Min. & Chem. May Brothers, Inc. *# Magcobar Baroid Div. National Lead Co. *# *# #Drilling Specialties Co. Milwhite Mud Sales Co. Milwhite Mud Sales Co. Brown Mud Co. #Westvaco Superbar Sales Superbar Sales Superbar Sales Superbar Sales Superbar Sales Baroid Div. National Lead Co. Baroid Div. National Lead Co. Milwhite Mud Sales Co. Magcobar Black Hills Bentonite TSPP T-8 Uni-Cal Uni-Gel Viz-Thin Workover Clay Wyo-Jel 200 X-Cor XP-20 Treat sodium pyrophosphate Shale control mud Modified alkyl aryl sulfonate Wyoming bentonite Ferro-chromelignosulfonate Low yield workover clay Bentonite Corrosion inhibitor Chrome Lignite ##Blockson Chemical Magcobar Milwhite Mud Sales Co. United Engineering Corp. #Crown Zellerbach Corp. Milwhite Mud Sales Co. Archer-Daniels-Midland Baroid Div. National Lead Co. Magcobar

Description

Maker or Distributor

Product Trade Name

Description

Maker or Distributor

Redwood bark extract Modified lignosulfonate California clay Treated lignite Pyrophosphate

Palcotan 950 Peltex P-95 Polytone Pyro, Anhydrous Paraformaldehyde Preservative Phosphate QBT Q-Broxin Q-X Quebracho compound Quebracho Qualex

Paraformaldehyde Complex phosphates Quebracho-based thinner Ferrochrome lignosulfonate Quebracho compound

Quick-Gel Ray Flo RD 111 Ranger Pure Quebracho Sapp Spersene Shale-Ban Soda Ash Sodium Bichromate Soltex Super-Col Superligco Shale-Rez Sodaphos Superben Superyield Super Quebracho Super Thin Super Starch Smentox

Tannex

Quebracho Sodium carboxymethylcellulose Extra high yield bentonite Hemlock extract Processed lignosulfonate Preu Quebracho Sodium acid pyrophosphate Chrome lignosulfonate Shale control compound Soda ash Sodium bichromate Mud lubricant Extra high yield bentonite Caustic lignite High pressure lubricant Phosphate Wyoming bentonite Sub-bentonite Quebracho mixture Mineral lignite Pregelatinized starch Cement contamination treating agent Quebracho compound Afrox Atlas Corrosion Inhibitor 100 Am-9 G-2 Gafen Fa-1

Tanco Tannathin Tower-Gel

Quebracho compound Lignite Wyoming bentonite

Treat Causticized lignite Atlas Mud Co. ___________________________________________________________________________

#Several distributing companies

*Several packaging companies

68

Table 4. Materials for Drilling Fluid Systems (cont.)

Invert Emulsion and Oil Muds (cont.) Product Trade Name Description Maker or Distributor
Antara Chemical Halliburton Co. Halliburton Co. Halliburton Co. #Monsanto Chemical #Proctor & Gamble Mud Control Laboratories #Union Carbide Chemicals #Union Carbide Chemicals #Union Carbide Chemicals Well Completions, Inc. Well Completions, Inc. Well Completions, Inc. Well Completions, Inc. No-Bloc Special Additive 47 Special Additive 58 Therm-Oil Atlas Mud Co. Oil Base, Inc. Oil Base, Inc. Oil Base, Inc. Oil Base, Inc. Mud Control Laboratories Mud Control Laboratories Baroid Div. National Lead Co. Baroid Div. National Lead Co. Baroid Div. National Lead Co. Oil Base, Inc.

Air/Gas Drilling Materials (cont.) Description Maker or Distributor Product Trade Name

Gafen Fa-7 Halliburton-Sorb Howco-Suds Hydro-Lok Oilfos OK Liquid Synfoam Tergitol NP-35

Tergitol NPX

Tergitol TMN

Well-Foam FS Well-Foam 3 Well-Foam 917 Well-Parch

Foaming agent, fresh & saline Water absorbing agent Surfactant, foaming agent Water Shutoff plastic slurry Deflocculating agent Foaming Agent Foaming Agent Nonyl phenyl polyethylene glycol ether Nonyl phenyl polyethylene glycol ether Trimethyl nonyl ether of polyethylene glycol Foaming agent Foaming agent Corrosion inhibitor Dryin and anti-ballin agent Magcobar Magcobar Oil Base, Inc. Oil Base, Inc. Milwhite Mud Sales Co. Low Solids Muds Pregelatinized starch Capryl alcohol Non-ionic surfactant Anionic surfactant Alpine Mud Service Milwhite Mud Sales Co. Atlas Mud Co. Atlas Mud Co.

Invertin Jel-Oil Ken Oil Ken-X Concentrate 1 Ken-X Concentrate 2 Ken-X Concentrate 3 OB Mixfix OB Gel Petrotone Peptomagic Perm-Base Perm-Wate Protectomagic Protecto-Mul

Emulsifier Oil mud Oil mud Invert Emulsifier Stabilizer (weight) Stabilizer (temperature) Viscosity reducer To increase viscosity Oil mud suspending agent Crude oil-based fluid Oil mud concentrate Calcium carbonate Oil dispersed asphalt Concentrate for invert emulsion Invert emulsion fluid To improve suspension properties To improve suspension, gel properties Invert Emulsion concentrate

Dowell Div., Dow Chemical Magcobar #Ken Corp. #Ken Corp. #Ken Corp. #Ken Corp. Oil Base, Inc. Oil Base, Inc. Baroid Div. National Lead Co. Oil Base, Inc. Macco Corp. Macco Corp. Oil Base, Inc.

Invert Emulsion and Oil Muds

Atlas-Invert 400 Black Magic Supermix Black Magic Premix Chemical V

Chemical W Control Invert Control Emulsion Oil Driloil

Polyoxyethylene product Fluid for high temp. wells Oil fluid, not high weight Additive to Black Magic, improve gel Treating agent for Black Magic Oil mud concentrate Nonionic surfactant Oil mud concentrate Loloss Lube Flow Mac-O-Mul Mudfloc Separan

Alloid Anti-Foam Atlas Emulso 500 Atlas Drilling Surfactant Atlasfloc Barafloc Drilltex Driscose

Atlas Mud Co. Baroid Div. National Lead Co. #T. M. Duche & Sons, Inc. #Drilling Specialties Baroid Div. National Lead Co. #Gibralter Minerals Macco Corp. Mud Control Laboratories Milwhite Mud Sales Co.

Driltreat Duratone Economagic

Oil mud stabilizer Oil mud filtration control agent Crude-oil based completion fluid

E-Z Mul

Baroid Div. National Lead Co. Emulsifier for CaCl solutions in oil Geltone Oil mud gelling agent Baroid Div. National Lead Co. Hot Lime Varifat lime *# Invermul Oil mud emulsifier Baroid Div. National Lead Co. ___________________________________________________________________________
#Several distributing companies

Flocculating gum Clay flocculant Guar gum Sodium carboxymethylcellulose Gum Guar Shale control Non-ionic surfactant, emulsifier Highly active flocculating agent Flocculating agent

*Several packaging companies

69

Table 4. Materials for Drilling Fluid Systems (cont.)

Maker or Distributor
*# Atlas Mud Co. Atlas Mud Co. Atlas Mud Co. Controlbar Dri-Job Drilling bar G-7 Super Weight Galena Invertin Wate Maccowate Magcobar Maybar Mil-Bar OB Hevywate OB Wate Superbar Uni-Bar Yuba Barite Barite Barite Barite Barite Barite Barite Barite Barite Calcium carbonate Barite Low gravity barite Barite Iron-arsenic compound Lead sulfide Acid-soluble material Baroid Barite Atlas Bar Barite Atlas Mud Co. Baroid Div. National Lead Co. Mud Control Laboratories Macco Corp. Drilling Mud, Inc. Magcobar Baroid Div. National Lead Co. Dowell Div., Dow Chemical Macco Corp. Magcobar May Brothers Milwhite Mud Sales Co. Oil Base, Inc. Oil Base, Inc. Superbar Sales United Engineering Corp. Yuba Milling Div. Ala-Bar Albar Barite (barium sulfate) Barite Alamo Lumber Co. Alpine Mud Service

Product Trade Name

Surface Active Agents Description Product Trade Name Maker or Distributor

Weighting Materials Description

Aluminum stearate Anionic surface active emulsifier Petroleum sulfonate

Aluminum Stearate Atlas Drilling Surfactant 100 Atlas Drilling Surfactant 200 Atlas Drilling Surfactant 300 Atlas Cmulso 500 Atlosol Ceox Con Det Control M-D Control Emulsion Oil

Nonionic surfactant

Nonionic surfactant Atlas Mud Co. Mixed esters #Atlas Chemical Industries Soluble oil-type surfactant Mud Control Laboratories Anionic detergent Baroid Div. National Lead Co. Low solids, mud additive Mud Control Laboratories Anionic surface active Mud Control Laboratories emulsifier Control Flow Oil-soluble surfactant Mud Control Laboratories Controlsol Nonionic surfactant and Mud Control Laboratories emulsifier D-D Mud detergent Magcobar Drilling Milk O/W Emulsifier Magcobar Drill Lube Surfactant, EP lubricant #Mud Engineering Supplies DME For compounding surfactant #Antara Chemicals muds Emulsifier F Nonionic surfactant #Mud Engineering Supplies Emulsifier S Nonionic surfactant #Mud Engineering Supplies Maco-Mul Nonionic surfactant, Macco Corp. emulsifier Maco-Lube Surfactant, EP lubricant Macco Corp. Magconate Petroleum sulfonate Magcobar Milwhite M-D Low-solids mud additive Milwhite Mud Sales Co. Mil-Olox Vegetable oil soap Milwhite Mud Sales Co. Olox Neutralized soap #Dril-Kem, Inc. Santomerse Sodium alkyl aryl sulfonate #Monsanto Chemical Seeco-Mul Vegetable oil soap #Crossett Chemicals Trimulso Emulsifier Baroid Div. National Lead Co. White Magic Non-Fluorescing emulsifier Oil Base, Inc. ___________________________________________________________________________
#Several distributing companies

*Several packaging companies

70

Table 4. Materials for Drilling Fluid Systems (cont.)

Maker or Distributor
Leather Seal Leath-O Magco-Fiber Magco-Mica Masterbridge Masterplug Masterseal Mayfiber Mayflakes Maymica Micatex Mil-Cedar Plug Mil-Fiber Milflake Milmica Mil-Plug Mil Seal Mil-Wool Mud Fiber Mica Nut Plug Oil Patch Palco Seal Pheno-Seal Polyflake Poly-Plug Poz-Plug Plug-Git Plastic Seal Rubber Seal Sealflakes Silvacel Stop-It Strata-Seal Super Fiber Super Seal Super Mica Superbridge Tuffernell Wall-Nut Walnut Plug Lather fibers Leather fibers Shredded wood fiber Graded mica Extra-course almond shells Shaped rubber Almond shells Cane, wood fiber blend Shredded cellophane flakes Grade mica Mica Cedar wood fibers Sugar cane bagasse Shredded cellophane flakes Graded mica Pulverized walnut shells Wood chips Fibrous mineral wood Cane fibers Sized mica Ground walnut shells Ground walnut shells Processed redwood fibers Ground plastic Oil soluble film Fibers and plastic Wood chips Wood fibers Ground formica Ground rubber Fragmented cellulose Fir and balsum fiber Cedar wood fibers Expanded perlite Cane, wood fibers Shredded cellophane flakes Graded mica Expanded perlite Walnut shells Nutshells Walnut shells Baroid Div. National Lead Co. Milwhite Mud Sales Co. Magcobar Magcobar Masterseal Sales Corp. Masterseal Sales Corp. Masterseal Sales Corp. May Brothers May Brothers May Brothers Baroid Div. National Lead Co. Milwhite Mud Sales Co. Milwhite Mud Sales Co. Milwhite Mud Sales Co. Milwhite Mud Sales Co. Milwhite Mud Sales Co. Milwhite Mud Sales Co. Milwhite Mud Sales Co. Magcobar #U.S. Mica Co. Jolex Mica Magcobar Mud Control Laboratories #Pacific Lumber Co. # Baroid Div. National Lead Co. Cherokee Laboratories #Poz-Plug Corp. Baroid Div. National Lead Co. Alamo Lumber Co. Atlas Mud Co. Mud Control Laboratories #Wayerhauser Timber Co. #Texas Cedar Seal Co. #Great Lakes Carbon Corp. Superbar Sales Superbar Sales Superbar Sales Mud Control Laboratories Macco Corp. Baroid Div. #Dugdale & Sons National Lead Co.

Product Trade Name

Lost Circulation Additives Description Product Trade Name

Lost Circulation Additives (cont.) Description Maker or Distributor

Ala-Fiber Ala-Flake Ala-Mica Ala-Plug Alseal Atlas Fiber Atlas Mica Ala-Shell Alflake Alpine Mica Aspen Fiber Bark-Seal Beaver Dam Bristex Bristex-Seal Cel-Flakes Cell-O-Phane Cell-O-Seal Cedar Seal Cert-N-Ceal

Fibrous material Alamo Lumber Co. Shredded cellophane flakes Alamo Lumber Co. Shredded mica Alamo Lumber Co. Graded walnut shells Alamo Lumber Co. Cane, wood fiber blend Alpine Mud Service Sugar cane bagasse Atlas Mud Co. Sized mica Atlas Mud Co. Pecan shells Alamo Lumber Co. Shredded cellophane flakes Alpine Mud Service Graded mica Alpine Mud Service Aspen fibers #Aspen Fiber Co. Shredded tree bark Alpine Mud Service Ground gilsonite Gibralter Minerals Hog bristles #Bristex Co. Hog bristles and cotton lint #Bristex Co. Ground cellophane United Engineering Corp. Shredded cellophane flakes #Arnold & Clarke Shredded cellophane flakes Magcobar Cedar fiber #Dril-Kem, Inc. Delayed action bentonite, gran. Mat. #Macco Corp. Chek-Loss Sized neoprene rubber Milwhite Mud Sales Co. Chip-Seal Shredded wood fiber Magcobar Control Fiber Fibrous material Mud Control Laboratories Control Wood Acid-soluble mineral wood Mud Control Laboratories Cottonseed Hulls Cottonseed hulls *# Chemical W Agent to form gel pills Oil Base, Inc. Chrome Leather Shredded leather Alamo Lumber Co. Dicks Mud Seal Ground naner #Dicks Mud Seal Co. Feather Stop Feathers Milwhite Mud Sales Co. Fiber-Seal Blended fibers Magcobar Fibertex Cane fibers Baroid Div. National Lead Co. Formaplug Clay-cement Magcobar Formaseal Air blown asphalt Oil Base, Inc. Flaxseal Ground flax shive Archer-Daniels-Midland Hy-Seal Ground paper Baroid Div. National Lead Co. Jelflake Cellophane flakes #Dowell Div. Dow Chemical Ko-Seal Granulated corn cobs Mud Control Laboratories King Seal Textile fibers Alamo Lumber Co. Krevice Klog Drop bags of granular bentonite Baroid Div. National Lead Co. Leather Floc Leather fibers Magcobar ___________________________________________________________________________
#Several distributing companies

*Several packaging companies

71

APPENDIX B

CEMENT ADDITIVES

72

CEMENT ADDITIVES1
Cement additive materials may be classified as follows: 1. Extenders 2. Accelerators 3. Retarders 4. Weighting Materials 5. Lost Circulation Control 6. Dispersants 7. Water Loss Control 8. Special Materials

Extenders

The use of extenders in cement has allowed the reduction of the slurry density, increase in the slurry yield, and reduction of cost. Water is the primary extender; however, if the recommended water content of the cement is exceeded, there is free water. The addition of extenders will alleviate this problem. Another reason for using extenders in cement is to reduce the hydrostatic pressure on the formation. The widely used extenders are: 1. Bentonite (montmorillonite) 2. Natural Pozzolan 3. Artificial Pozzolan (Flyash) 4. Perlites (Expanded) 5. Diatomaceous Earth 6. Sodium Silicate 7. Kolite and Gilsonite
Bentonite

Bentonite or commonly referred to as gel may be dry blended with the cement or prehydrated in the mix water. The API recommended water is 5.3% for each 1% bentonite added to the dry cement. If the bentonite is prehydrated in the mix water, you may use one fourth the amount of bentonite dry blended (that is 1:4 ratio). Bentonite may be used from 2 to 25% by weight of cement; however, it is normally used in the range of 2 to 16%. Table 5 shows the effect of bentonite on the slurry properties of typical Class H cement.
1

Calvert, D.B., Cementing Materials, Cementing Symposium, Ardmore, OK, May 1977..

73

Table 5. Effect of bentonite on the slurry properties of Class H cement (using 38% water by weight of cement)
Bentonite (%) Water Content (gal/sk) 0 4.29 2 5.49 4 6.69 8 9.07 12 11.48 Slurry Weight (lb/gal) 16.45 15.4 14.7 14.1 12.9 Slurry Yield (Cu ft/sk) 1.05 1.22 1.39 1.56 2.08

The addition of bentonite reduces the compressive strength and normally will reduce the thickening time.
Natural Pozzolan

Natural pozzolans have been used for a number of years blended with cement and bentonite to design reduced weight cement systems. It is used primarily in the California operations.
Artificial Pozzolan (Flyash)

Artificial pozzolan or flyash as its commonly referred to has been used widely in the cementing operations. It normally is blended with cement and bentonite to develop the lightweight systems.
Perlite (Expanded)

Perlite is a volcanic material that is crushed and then heated to expand it. Perlites were widely used in field operations; however, it is used very little today.
Diatomaceous Earth

Diatomaceous earth is a special grade of material that may be used to design low density cement systems. It normally is used at a concentration of 10 to 40% by weight of cement. A density of about 11 lb/gal using 40% diatomaceous earth by weight of cement.
Sodium Silicate

Sodium silicate has been used in the past few years as a lightweight material because it allows for large quantities of water to be added while using only small amounts of the additive. It normally is used at a ratio of 1 to 3% by weight of cement.
Kolite and Gilsonite

Kolite is a graded coal whereas gilsonite is an asphalt material. They both may be used to reduce the density; however, their primary use is as a lost circulation material.

74

Accelerators

Accelerators are normally used at low temperature conditions to accelerate the thickening time and increase the early strength development of the cement. The commonly used accelerators are: 1. Calcium chloride 2. Sodium chloride 3. Calcium sulfate 4. Sodium silicate
Calcium Chloride

Calcium chloride is the most widely used cement accelerator used in field operations. It is used normally at a concentration of 2 to 4% by weight of cement. It may be added to the dry cement or it may be mixed in the mix water. Calcium chloride does not affect the ultimate compressive strength of the set cement. Table 6 shows the effect of calcium chloride on strength development of set cement.
Table 6. Effect of Calcium Chloride on Set Cement
Calcium Chloride (%) 0 2 60F 6 hrs. Not set 140 12 hrs. 80 650 6 hrs. 60 350 80F 12 hrs. 450 1190 6 hrs. 425 1350 110F 12 hrs. 925 2500

Sodium Chloride

Sodium chloride is also an effective accelerator for cement systems. It normally is used at a concentration of 3 to about 10% by weight of mix water to obtain total acceleration. It should also be noted that at high concentrations (20% by weight of water) sodium chloride becomes a retarder.
Calcium Sulfate

The himihydrate form (plaster of paris) is the most common calcium sulfate used. It may be used up to 100% by weight of cement. Very short thickening times may be obtained with these systems.
Sodium Silicate

The DiacelR cement systems developed by Phillips is the primary use of sodium silicate as an accelerator. It is used mainly when CMHEC (carboxmethyl hydroxyethyl cellulose) water loss control material has been added to the system.
R

Trademark

75

Retarders

Retarders are used in cement systems where bottomhole temperatures are such that adequate thickening times cannot be obtained with neat cements. Retarders should be compatible with other additives that might be used in cement systems. Retarders are designed not only to retard the set of cement, but they may function to increase or decrease viscosity. The common retarders are: 1. Lignin materials 2. Organic blends 3. Celluloses 4. Inorganic materials
Lignin

Lignin is the retarder most commonly used. They are effective over a wide range of temperature; however, without a retarder supplement, they are not used at bottomhole circulating temperatures above about 200F. The lignin will also reduce slurry viscosity. Normal use is from 0.1 to 1.0% by weight of cement depending on the class of cement. Table 7 shows the effect of lignin retarder on a Class H cement system.
Table 7. Effect of Lignin Retarder on a Typical Class H Cement
Retarder (%) Thickening Time (hours: min) API Casing Cementing Tests for Simulated Well Depth (ft) of: 8,000 10,000 12,000 14,000

0.0 0.2 0.3 0.4

Organic Materials

1:56 2:15 3:38 4:42

1:26 2:12 2:40 3:36

1:09 1:38 2:14 3:10

1:00 1:25 1:58 2:58

The organic retarders are offered to the industry by all the service companies. Most of these retarder systems are property in nature and the cement systems are designed for specific well conditions.
Celluloses

Cellulose materials were initially developed as water loss control materials for cement; however, it is also found that retardation could also be obtained with these materials. A secondary function of the cellulose materials is that they will increase the viscosity of the slurry. The most common cellulose used is CMHEC.

76

Inorganic Materials

Saturated sodium chloride water or salt saturated cement is the most common inorganic retarder used. Salt saturated cements retard over a wide temperature and at low temperatures may cause extended thickening times. Formation properties will normally determine salt concentration.

Weighting Materials

In some areas, normal cement densities are not capable of controlling down hole well conditions. An increase in the slurry density will require the addition of a weighting material. An acceptable weighting material should not (1) affect the overall properties of the slurry, (2) not interfere with well operations and (3) be chemically inert. The most common weighting materials are: 1. Hematite (Iron oxide) 2. Ilmenite (Iron - titanium oxide) 3. Barite (Barium sulfate)
Hematite

Hematite is an iron oxide with a specific gravity of approximately 5. It is the most widely used weighting agent in field operations. It is used at a concentration of about 5 pounds to 50 pounds per sack of cement depending on well conditions. It is in the fine to semi-fine particle size range and may require additional mix water to be added.
Ilmenite

Ilmenite is an iron-titanium oxide with a specific gravity of approximately 4.6. It is used from about 5 pounds to 50 pounds per sack; however, it is considered to be a coarse ground particle and slurry properties should be considered.
Barite

Barite is a fine grind barium sulfate with a specific gravity of approximately 4.3. Barite is not widely used in cement slurry design today because of its fine grid and high water requirement.

Lost Circulation Control

Lost circulation or loss of returns is a problem that is encountered in cementing operations during placement of slurry in fractured zones (either natural or induced) and/or cavernous type formations. Lost circulation may be controlled in different ways; however, a reduction in slurry 77

density combined with a budging material and many times a flake material is effective. The most common lost circulation materials are: 1. Kolite 2. Gilsonite 3. Cellophane flakes
Kolite

Kolite is a graded coal that has been prepared as an aid in lost circulation. It may be used over a concentration range of 1 to 25 pounds per sack, but common use range is 5 to 20 pounds. Kolite does require that additional water be used for mixing and for each 25 pounds of kolite, an additional one gallon of mix water should be used.
Gilsonite

Gilsonite is an asphalt material which is mined and graded to a specific particle size range to aid in lost circulation control. It may be used at a concentration of 5 to 50 pounds per sack. Normal usage range is 5 to 25 pounds. The water requirement for gilsonite is for each 25 pounds added to the system, an additional one gallon of water should be used.
Cellophane Flakes

Cellophane flakes are used in conjunction with the granular type materials to aid in building a bridging system. They are normally used at a concentration of to pound per sack of cement. There are also a number of specialty cement systems designed to aid in lost circulation control. The most common are (1) Gypsum cement (Calseal or Gypseal), (2) Gypsum - Portland cement blends, (3) gel cement and (4) Diesel oil - cement or diesel oil - bentonite blends. Well conditions in most cases will indicate which system may be best to solve the lost circulation problem.

Dispersants

The use of dispersants allowed the application of turbulent flow cementing be performed at practical pump rates. Slurries containing dispersants have a reduced viscosity which allows lower pressures on the formation during placement of the slurry. The common dispersants are: 1. Alkyl aryl sulfonates (powder and liquid) 2. Lignin 3. Inorganic salts 4. Organic acids 78

Alkyl aryl Sulfonates

The sulfonates are the most widely used dispersants because of the wide temperature range and overall effect on slurry properties. Another major benefit of dispersants in cement is the ability to design reduced water or densified cements. Typical Class H cement may be increased in weight to about 17.5 pounds per gallon using a dispersant and no weighting material. Table 8 shows the effect of a sulfonate dispersant or critical pump rate (Qc) at given well conditions.
Table 8. Effect of sulfonate dispersant or critical pump rate (Qc)
Cement System Class H cement Class H cement Pozzolan: Cement Blend Pozzolan: Cement Blend Dispersant (%) 0 1.0 0 1.0 Critical Pump Rate, Qc 4-1/2 Pipe in 7-7/8 Hole 17 BPM 4 BPM 22 BPM 5 BPM

The sulfonate dispersants are compatible with most cement materials; however, salt concentrations (greater than 18% by weight of water) will have a detrimental effect and should be tested before use.
Lignin

Lignins have a thinning effect on many cement systems; however, they also retard at low temperatures and, therefore, are limited somewhat in their overall use. The most common use of lignin as dispersants is in the high-gel cement systems.
Inorganic Salts

Sodium chloride is the most common inorganic salt used as a dispersant. It is most effective in the pozzolan; cement blends, bentonite and diatomaceous earth systems.
Organic Acids

Organic acids are used primarily as retarders in cement; however, they will also show a thinning effect on many cement systems. Well conditions will dictate their use in most cases.

Water Loss Control Materials

A neat cement system when tested under API conditions (Fluid Loss) will show a 30-minute loss of greater than 1000 cc. The loss of cement filtrate may cause formation damage, premature setting of the cement, inability to place the cement, and unsuccessful squeeze cement operations. A water loss control material allows for the development of a filter cake on the formation face, thereby control of the slurry properties. The most common materials are:

79

1. Cellulose materials 2. Polymers (Liquid)

Cellulose materials

The cellulose materials are the most widely used in water loss control. They are effective in most cement systems used in the field. Their usage range will vary from 0.5 to 1.5% by weight of cement. Cellulose presently used may be affected by the common inorganic salts (calcium chloride, sodium chloride and potassium chloride).
Polymers (Liquid)

A very effective water loss control material was introduced in the late 1960s which must he added to the mix water. It is effective over a wide temperature range and has little effect on the slurry properties from the standpoint of thickening time and compressive strength. It is normally used in the range of 0.1 to 0.5 gallons per sack of cement.

Special Materials

There are a number of additives that are used in cement slurry design to build specific properties. Mud decontaminates are used to decrease the effect of lignin type muds on the set properties of the cement. They are normally used at a concentration of 1.0% by weight of cement. The use of fine silica (silica sand and silica flour) is normally added to a cement system which is to be exposed to high temperatures (may vary depending on cement system) to prevent loss of strength. Fine silica is compatible with all API cements and normally will be used as a concentration of 20 to 40% by weight of cement. Additional water is usually required for mixing when fine silica is used. There are other materials which have application such as latex, radioactive tracers, fibers, special lightweight cements, expanding cement, washes, spacers, and antifoam materials. There is considerable information developed by the service companies in regard to the properties of the cementing materials that are discussed in this article. Some of the materials may vary in chemical nature; however, they are designed to perform for your specific well conditions. Attached is one of the most recent comparative listings of cement materials used by the cementing service companies.

80

Table 9. CEMENT PRODUCT COMPARISON - CHARTCOMPETITIVE EQUIVALENTS

Halliburton Dowell B.J. Weslan Production Description

Classification

Magcibar

Accelerators

Retarders

Fluid Loss Additive

Turbulence Inducers

H-TLW Blends Extenders

Anti-Foam Agents

Thixotropic Cement Silica Sand

Weighting Material

Spacers & Washes

Lost Circulation

Mud Decontaminant

Latex

CaCl2 MCA-L MA-2 Diacel A Salt MLR-1 HLR-3 MHR-8 MHR-9 MFLR-7 MHR-600 MLR-L MHR-L MFL-4 MFL-5 MFLR-7 MFL-L MCD-3 MCD-4 MCD-L Multidense M-Gel Gilsonite Thrifty Mix Thrifty Mix-L Magco Poz A Magco Pox 180 Econoblend MFP-5 MFP-L Thixocem MS-1 MS-2 Nagcobar MW-2 MW-1 MHW-1 MCS-2 MCS-3 Gilsonite Cello-Seal Kwik-Seal Nut Plug Hard-Set 1 Hard-Set II MCL-2

CaCl2 CaCl2 HA-5 Diacel A Salt HR-7 HR-4 HR-12 HR-15 Diacel LWL HR-20 HR-6L HR-13L Halad 9,14 Halad 9,14 Diacel LWL CFR-2, LA-2 CFR-2 CFR-1 CFR-2 1:1 H-TLW Howco Gel Gilsonite Econolite Econolite-L Pozmix A Pozmix 140 Howcolight NF-P D-Air 2 Thixomix Silica Flour Silica Flour Coarse Barite Hi-Dense 3 Hi-Dense 2 Mud-Flush SAM-4,5 SMA-4,5 Gilsonite Flocele Walnut Shells Mud Kil-1 Mud Kil-2 LAP-1

S-1 D-77 D-43 D-57 D-44 D-13 D-28 D-93 D-8 D-99 D-81 D-60 D-59 D-8 D-73 TIC II D-45 TIC I D-65 D-80 1:1 H-TLW Bentonite D-24, D-92 D-79 D-75 Litepoz 3 Litepoz 180 Litepoz 300 D-46 D-47 Reg. Fill-up D-66 D-30 D-31 D-76 D-18 CW-7, CW-100 Spacer 1000 Oil Base Spacer D-24 D-29 Kwik-Seal D-42 K-21 K-21 D-15

A-7 A-7L A-B Diacel A A-5 Kembreak R-5 R-11 M-6 R-6 R-14L R-14L D-19 D-22 R-6 D-31 D-31-L 1:1 H-TLW BJ Gel D-7 A-2 A-3L Diamix F Thermosset D-6 D-21 Thixotropic D-8 D-SC W-1 W-5 W-3 Mud-Clean Mud-Sweep Oil Base Mud Sweep D-7 Cello-Flake Kwik-Seal Tuf-plug Firm Set I Firm Set II D-5

CaCl2 WA-4 Diacel A Salt WR-1 WR-2 WR-6 WR-7 Diacel LWL WR-L1 CF-1 CF-2 Diacel LWL TF-4 TF-5 Talc Bentonite Gilsonite Thrifty-Lite Fozment A Thriftyment AF-8 AF-L Thixoment SF-3 SF-4 Barite WM-2 Ilmenite WMW-1 APS-1 APS-1 Gilsonite Cell-O-Seal Kwik-Seal Tuf-plug Shur Set I Shur Set II CLX-1

Calcium Chloride Liquid Accelerator Inorganic Accelerators Sodium Silicate Sodium Chloride Low Temperature Retarder Low Temperature Retarder High Temperature Retarder High Temperature Supplement Diacel LWL CMHEC Extreme High Temperature Low Temperature Liquid Retarder High Temperature Liquid Retarder Fluid Loss Control Additive Fluid Loss Control Additive Diacel LWL CMHEC Liquid Fluid Lost Additive Cement Dispersant Cement Dispersant Liquid Cement Dispersant Various H-TLW Blends Cementing Grade Bentonite Extender and Lost Circulation Chemical Extender Liquid Chemical Extender Artificial Pozzolans Pozzolan Lime Mixtures Class II-Poz Blends Powdered Antifoam Agents Liquid Antifoam Agents Thixotropic Cement Slurries Minus 200 Mesh Silica Flour Oklahoma #1 Sand Barite Hematite Ilmenite Mud Thinner-Spacer Water Based Mud Spacer Oil Based Mud Spacer Granular Natural Hydrocarbon Cellophane Flakes Graded Particle Sizes Ground Walnut Shells Mud Kill Patented by Gulf Oil Mud Kill Patented by Gulf Oil Latex Additive

81

APPENDIX C

RESULTS AND DATA SHEETS

82

Date: PNG 451 - OIL WELL DRILLING LABORATORY DATA SHEET 1

Experiment #1: Properties of fresh water muds

Group No.: 3) 4)

Group 1) Members: 2)

Group No.
Reading (sec) 10 rpm 50 rpm 100 rpm

Mud Mud balance (ppg) No.

Marshall Funnel

Rheometer (lb/sq. ft.)

200 rpm 300 rpm 600 rpm

Gel strength (lb/sq. ft.)

10 sec 10 min

C.F.

83

Date: PNG 451 - OIL WELL DRILLING LABORATORY DATA SHEET 2

Experiment #1: Properties of fresh water muds

Group No.: 3) 4)

Group 1) Members: 2)

Group No.
V1 V2 V3 V4 V5 V6 V7 V7.5 V10

Mud No.

pH

Filter press loss (ml)

V15 V20 V25 V30

Cake thick.
(in)

Mud resistivity (ohm-m)

Mud Filtrate Cake

Spurt

84

PNG 451 - OIL WELL DRILLING LABORATORY RESULT SHEET Group No.: 3) 4)
Apparent Viscosity (cp) 10 rpm 50 rpm 100 rpm 200 rpm 300 rpm 600 rpm Mud density (ppg) Plastic viscosity (cp) Yield point (lb/ft2)

Experiment #1: Properties of fresh water muds

Group 1) Members: 2)

Group No.

Mud No.

2
Gel strength (lb/sq. ft.) 10 sec 10 min pH Mud resistivity Mud Filtrate (ohm-m) Cake 30-min fluid loss (ml) Cake thickness (1/32's in)

Group No.

Mud No.

2
85

Date: PNG 451 - OIL WELL DRILLING LABORATORY DATA SHEET 1

Experiment #2: Effects of sodium salts on fresh water muds

Group No.: 3) 4)

Group 1) Members: 2)

Group No. Rheometer (lb/sq. ft.)

100 rpm 300 rpm 600 rpm 10 sec 10 min Reading

Mud Mud balance (ppg) No.

Gel strength (lb/sq. ft.)

Cake thick.
(in)

pH

C.F.

4
86

Date: PNG 451 - OIL WELL DRILLING LABORATORY DATA SHEET 2

Experiment #2: Effects of sodium salts on fresh water muds

Group No.: 3) 4)

Group 1) Members: 2)

Group No.
V1 V2 V3 V4 V5 V6 V7 V7.5 V10 V15 V20

Mud No.

Filter press loss (ml)

V25 V30

Mud resistivity (ohm-m)

Mud Filtrate Cake

Spurt

4
87

PNG 451 - OIL WELL DRILLING LABORATORY RESULT SHEET Group No.:

Experiment #2: Effects of sodium salts on fresh water muds 3) 4)

Plastic viscosity (cp) Gel strength (lb/sq. ft.) 10 sec 10 min pH 30-min fluid loss (ml) Yield point (lb/ft2) Cake thickness (1/32's in)

Group 1) Members: 2)

Group No.

Mud No.

Mud density (ppg)

Mud resistivity (ohm-m) Mud Filtrate

1 2 3 4

1 2 3 4

1 2 3 4

88

Date: PNG 451 - OIL WELL DRILLING LABORATORY DATA SHEET 1

Experiment #3: Viscosity reducing agents

Group No.: 3) 4)

Group 1) Members: 2)

Group No.
Reading 300 rpm 600 rpm 10 sec 10 min
Spurt

Mud Mud balance (ppg) No.

Rheometer (lb/sq. ft.)

Gel strength (lb/sq. ft.)

V1 V2

Filter press loss (ml)

V3 V4 V5 V6 V7 V7.5

pH

C.F.

89

PNG 451 - OIL WELL DRILLING LABORATORY RESULT SHEET Group No.: 3) 4)
Mud density (ppg) pH Plastic viscosity (cp) Yield point (lb/ft2) Gel strength (lb/sq. ft.) 10 sec 10 min 30-min fluid loss (ml) Cake thickness (1/32's in)

Experiment #3: Viscosity reducing agents

Group 1) Members: 2)
Mud No.

Group No.

1 2 3 4 1 2 3 4 1 2 3 4

90

Date: PNG 451 - OIL WELL DRILLING LABORATORY DATA SHEET

Experiment #5: Regular cements, cement extenders and cement weighting materials

Group No.: 3) 4) Filter press loss (ml)

Spurt

Group 1) Members: 2)

Group No.
V1 V2 V3 V4 V5 V6

Cem Mud balance Rheometer Gel strength ent (ppg) (lb/sq. ft.) (lb/sq. ft.) No. C.F. Reading 300 rpm 600 rpm 10 sec 10 min
V7

V7.5

V10

3 Versa Tester Sample No.2

d1(in) d2(in) lbs. d1(in) d2(in)

Group No.

Sample No.3
lbs.

Cem ent Sample No.1 No. d1(in) d2(in) lbs. 1

91

PNG 451 - OIL WELL DRILLING LABORATORY RESULT SHEET

Experiment #5: Regular cements, cement extenders and cement weightinGroup No.: 3) 4)
Mud density (ppg) Plastic viscosity (cp) Yield point (lb/ft2) Gel strength (lb/sq. ft.) 10 sec 10 min Dehydratio n Time (min) 30-min Compressi fluid loss ve strength (ml) (psi)

Group 1) Members: 2)

Cement Group No. No.

1 2 3 1 2 3 1 2 4

92

Date: PNG 451 - OIL WELL DRILLING LABORATORY DATA SHEET

Experiment #6: Cement accelerators and retarders

Group No.: 3) 4) Filter press loss (ml)

Spurt

Group 1) Members: 2)

Group No.
V1 V2 V3 V4 V5 V6

Cem Mud balance Rheometer Gel strength ent (ppg) (lb/sq. ft.) (lb/sq. ft.) No. C.F. Reading 300 rpm 600 rpm 10 sec 10 min
V7

V7.5

V10

3 Versa Tester Sample No.2

d1(in) d2(in) lbs. d1(in) d2(in)

Group No.

Sample No.3
lbs.

Cem ent Sample No.1 No. d1(in) d2(in) lbs. 1

93

PNG 451 - OIL WELL DRILLING LABORATORY RESULT SHEET Group No.: 3) 4)
Mud density (ppg) Plastic viscosity (cp) Yield point (lb/ft2) Gel strength (lb/sq. ft.) 10 sec 10 min Dehydratio n Time (min) 30-min Compressi fluid loss ve strength (ml) (psi)

Experiment #6: Cement accelerators and retarders

Group 1) Members: 2)

Cement Group No. No.

1 2 3 1 2 3 1 2 4

94

Date: PNG 451 - OIL WELL DRILLING LABORATORY DATA SHEET

Experiment #7: Water loss additives and dispersants

Group No.: 3) 4) Filter press loss (ml)

Spurt

Group 1) Members: 2)

Group No.
V1 V2 V3 V4 V5 V6

Cem Mud balance Rheometer Gel strength ent (ppg) (lb/sq. ft.) (lb/sq. ft.) No. C.F. Reading 300 rpm 600 rpm 10 sec 10 min
V7

V7.5

V10

3 Versa Tester Sample No.2

d1(in) d2(in) lbs. d1(in) d2(in)

Group No.

Sample No.3
lbs.

Cem Sample No.1 ent No. d1(in) d2(in) lbs. 1

95

PNG 451 - OIL WELL DRILLING LABORATORY RESULT SHEET Group No.: 3) 4)
Mud density (ppg) 10 sec 10 min Plastic viscosity (cp) Yield point (lb/ft2) Gel strength (lb/sq. ft.) Dehydratio n Time (min) 30-min Compressi fluid loss ve strength (ml) (psi)

Experiment #7: Water loss additives and dispersants

Group 1) Members: 2)

Cement Group No. No.

1 2 3

1 2 3

1 2 4

96