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Drilling Fluids Manual

Section 3 Testing

Water-Based Drilling Fluids Testing Procedures

Mud Density
Mud Density is used to control subsurface pressures and stabilize the wellbore.
Mud density is commonly measured with a mud balance capable of ±0.1 lb/gal accuracy. A mud bal-
ance calibrated with fresh water at 70° ±5° should give a reading of 8.3 lb/gal.

Step

4. Measure and record the temperature of the sample of mud to be tested.

5. Place the mud balance base on a flat, level surface.

6. Fill the clean, dry, mud balance cup with the sample of mud to be tested. Rotate cap until it is firmly
seated. Ensure that some mud is expelled through the hole in the cap to remove any trapped air or
gas.

7. Place thumb over hole in cap and hold the cap firmly on the cup. Wash or wipe the outside of the
cup, and dry.

8. Place balance arm on the support base and balance it by moving the rider along the graduated
scale until the level bubble is centered under the center line.

9. Read the density (weight) of the mud shown at the left-hand edge of the rider and report to nearest
0.1 lb/gal. Enter result on API Drilling Mud Report as Weight (lb/gal, lb/ft 3) or Specific Gravity).

Marsh Funnel Viscosity

Marsh Funnel viscosity is used to indicate relative mud consistency or thickness.
Marsh Funnel viscosity is the time required (seconds) for a quart of mud to flow through a 2-in. long,
3/16-in. diameter tube at the bottom of the Marsh Funnel. This viscosity measurement is used to peri-
odically report mud consistency. One quart of water should flow through a Marsh Funnel in 26±
0.5 seconds.

Step

1. Hold one finger over the orifice at the tip of the funnel. Pour the mud sample through the funnel
screen until mud reaches the bottom of the screen (1500 cm3). Place viscosity cup beneath funnel
tip. Remove finger and start stop watch.

2. Stop the watch when the mud level reaches the 1-qt mark on the viscosity cup.

3. Record the number of seconds required to outflow 1-qt of mud. Enter on Drilling Mud Report as
Funnel Viscosity (sec/qt) API.

4. Measure and record temperature of mud sample to ±1°F.

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Rheology

Rheological properties measured with a rotational viscometer are commonly used to indicate sol-
ids buildups flocculation or deflocculation of solids, lifting and suspension capabilities, and to calcu-
late hydraulics of a drilling fluid.

A rotational viscometer is used to measure shear rate/shear stress of a drilling fluid - from which the
Bingham Plastic parameters, PV and YP, are calculated directly. Other rheological models can be
applied using the same data. The instrument is also used to measure thixotropic properties, gel
strengths. The following procedure applies to a Fann Model 35, 6-speed VG Meter.

Plastic Viscosity (PV) and Yield Point (YP)

Step

1. Obtain a sample of the mud to be tested. Record place of sampling. Measurements should be
made with minimum delay.

2. Fill thermal cup approximately 2/3 full with mud sample. Place thermal cup on viscometer stand.
Raise cup and stand until rotary sleeve is immersed to scribe lie on sleeve. Lock into place by turn-
ing locking mechanism (Figure 1).

Figure 1
Fann Model 35 6-Speed Viscometer

3. Place thermometer in thermal cup containing sample. Heat or cool sample to desired test temper-
ature of 115° ±2°F.

4. Flip VG meter toggle switch, located on right rear side of VG meter, to high position by pulling for-
ward.

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5. Position red knob on top of VG meter to the 600-rpm speed. When the red knob is in the bottom
position and the toggle switch is in the forward (high) position -this is the 600-rpm speed
(Figure 2).

Figure 2
Speed Selection Knob
(Caution: Change gears only when motor is running.)

6. With the sleeve rotating at 600-rpm, wait for dial reading in the top window of VG meter to stabilize
(minimum 10 seconds). Record 600-rpm dial reading.

7. With red knob in bottom position, flip the VG meter toggle switch to low position by pushing the tog-
gle switch away from you. Wait for dial reading to stabilize (minimum 10 seconds). Records
300-rpm dial reading. [See Step 8 to calculate the Plastic Viscosity and Yield Point].

8. The Plastic Viscosity and Yield Point are calculated from the 600-rpm and 300-rpm dial readings
as follows:

PV,cP =  600-rpm  –  300-rpm 

 dial reading  dial reading

YP,lb/100 ft 2 =  300-rpm  –  Plastic 

 dial reading  Vis cos ity

Gel Strength (10-sec/10-min)

Step

1. With red knob in bottom position, flip toggle switch to 600-rpm position (forward position). Stir mud
sample for 10 seconds.

2. Position red knob to the 3-rpm speed. When the red knob is in the middle position and the toggle
switch is in low (rear) position - this is the 3-rpm speed. Flip toggle switch to off position. Allow mud
to stand undisturbed for 10 seconds.

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3. After 10 seconds, flip toggle switch to low (rear) position and note the maximum dial reading. This
maximum dial deflection is the 10-second (initial) gel strength in lb/100 ft2. Record on the mud
check sheet.

4. Pull toggle switch to high and position red knob to 600-rpm speed. Stir mud for 10 seconds.

5. After 10 seconds, and while mud is still stirring, position red knob to the 3-rpm speed. Flip toggle
switch to off position and allow mud to stand undisturbed for 10 minutes.

6. After 10 minutes, flip toggle switch to low (rear) position and note the maximum dial reading. This
maximum dial deflection is the 10-minute gel strength in lb/100 ft2. Record on the mud check
sheet.

Static Filtration Tests

Control of filtration properties of a drilling fluid can be useful in reducing tight hole conditions and
fluid loss to formations.

Static filtration tests are used to indicate filter cake quality and filtrate volume loss for a drilling mud
under specific testing conditions. Filtration characteristics are affected by the types and quantities of
solids and their physical and chemical interactions. Temperature and pressure further affect these sol-
ids and their interactions.
To operate any equipment, manufacturer’s instructions should be carefully read. The following are gen-
eral instructions for a possible configuration of Low-Pressure/Low-Temperature Filtration and
High-Pressure/High-Temperature Filtration equipment. To operate any other units, manufacturer’s
instructions should be carefully read before attempting to perform testing.

Low-Temperature/Low-Pressure Filtration
1. Open main air valve by turning handle (located on lab bench) counter clockwise. Adjust regulator
to read 100 psi.

2. Be sure cell components, especially the screen, are clean and dry. Check gaskets and discard any
that are worn or distorted.

3. Assemble filtration cell (as illustrated in Figure 3). Lock cell bottom into position by turning cell
body until peg locks into J slot.

4. Pour mud sample to within 1/2 in. of top of cell. Place cell onto filter press rack.

5. Position cell lid onto top of cell body. To seal, turn filter press handle clockwise until hand-tight.

6. Place a clean, dry graduated cylinder under the drain tube of the filtration cell assembly.

7. Close bleeder valve. Maintain in the closed position while test is running (Figure 4).

8. Set interval timer for 30 minutes. Open valve located on filter press manifold by turning black knob
counterclockwise. Pull timer arm down and begin timing immediately.

9. At the end of 30 minutes, remove graduated cylinder. Measure and record filtrate volume collected.
Volume is measured in cm3 per 30 minutes. Close valve by turning black knob clockwise. Open
bleeder valve and release trapped line pressure.

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Figure 3
Low-Temperature/Low-Pressure Filtration Apparatus

Figure 4
Bleeder Valve

10. Turn filter press handle counterclockwise to remove filtration cell assembly from frame. Pour mud
back into viscosity cup, then carefully disassemble mud chamber.

11. Remove filter paper from screen, being careful not to disturb mud cake. Gently wash excess mud
from cake with a stream of water.

12. Measure and report thickness of filter cake to nearest 1/32 of an inch. Describe cake; i.e., soft,
tough, rubbery, firm, etc.

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High-Temperature/High-Pressure Filtration (HTHP)

To operate this or any other unit, manufacturer’s instructions should be carefully read before attempting
to perform testing. Extreme caution should be used in running this test. Equipment should be cleaned
and maintained in good working condition (Figure 5).

Figure 5
HTHP Filtration Unit

Step

1. Plug heating jacket cord into correct voltage for the unit.

2. Place metal thermometer in hole on outside from of heating jacket. Adjust thermostat and preheat
jacket to 10°F above desired test temperature.

3. While jacket is heating, check o-rings (3) on the following components and replace if worn or dis-
torted:

• High-Pressure Regulator
• Lid/Valve
• Cell Body

(See Figures 6, 7 and 8 for details.)

4. Stir mud sample 10 minutes with a high-speed mixer.

5. Close valve A by turning black knob clockwise.

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6. Turn handle counterclockwise on high pressure regulator, then load CO2 cartridge into chamber
(Figure 6).

Figure 6
Two Types of Puncture Pin Assemblies

7. Close valve B and pour stirred mud sample into cell, leaving 1/2 in. from the top lip to allow for
expansion. Position o-ring in groove inside cell body. Place filter paper on top of o-ring (Figure 7).

Figure 7
Assembly of Cell Body

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8. Open valve C and seat lid/valve assembly. Lubricate threads of allen screws with silicone grease
and tighten (Figure 8).

Figure 8
Assembled Cell Body

9. Close low-pressure shut-off valve.

10. Invert cell. (The lid/valve assembly is now at the bottom.) Carefully, install cell assembly into heat-
ing jacket.

Caution: The Heating Jacket is hot!

Transfer thermometer from the jacket to the thermometer well located on top of HTHP cell body
(Figure 9).

11. Slip high-pressure regulator (0-1500 psi) onto top of valve B and lock into place with steel ring.

12. Slip low-pressure regulator (0-200 psi) on bottom of valve C. Lock into place with steel ring. Be
sure bleeder valve on low-pressure regulator is in the horizontal (closed) position.

13. With valves B and C closed, apply 100 psi to both the high-pressure regulator and the low-pres-
sure regulator by turning regulator handles clockwise.

14. Open valve B. This is done to maintain 100 psi back pressure in the cell body while heating to the
desired temperature. Heating time should not exceed 1 hour (Figure 10).

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Figure 9
Cell Body Into Heating Jacket

15. When desired temperature is reached, increase pressure on high-pressure regulator to 600 psi by
turning regulator handle clockwise.

Note: If pressure on low-pressure regulator rises above 100 psi during the test, cautiously reduce
pressure by drawing off a portion of filtrate using valve D located on bottom of filtrate col-
lection chamber.

16. Open valve C. Start timer immediately at this point! Collect filtrate for 30 minutes, maintaining test
temperature within ±5°F (Figure 11).

17. At the end of 30 minutes close valve. Carefully open valve D and collect filtrate. Leave valve open
until low-pressure gauge reads 0 psi.

18. Note the total volume of filtrate, test temperature and pressure, and cell heat-up time. Because
most HTHP filter presses have a filter area of 3.5 in.2, the filtrate volume collected must be doubled
to correct to API standard 7.1 in.2 Calculate and record the API HTHP filtrate as follows:

API HTHP Filtrate = 2 ( cm 3 filtrate collected )

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Figure 10
Valve Positions During Heat-Up

Figure 11
Valve Positions During Filtration

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19. Unplug unit and allow cell and contents to cool to room temperature before proceeding to disas-
sembly procedure.

Note: CAUTION - Throughout the disassembly procedure, always assume there could be
trapped high pressure in the HTHP unit.

20. After HTHP cell assembly and contents are cooled to room temperature, proceed with disassem-
bly and cleaning procedure. Valves B and C should already be in the closed positions (Figure 12).

Figure 12
Valve Positions at End of Test

21. To bleed pressure from the high-pressure (top) regulator, be sure valve B is closed. Turn regulator
handle clockwise and carefully open valve A. Bleed pressure until CO2 cartridge is expended and
high-pressure gauge reads 0 psi (Figure 13).

22. To bleed pressure from the low-pressure (bottom) regulator, be sure that valve C is closed. Turn
regulator handle clockwise and carefully open valve D. Bleed pressure until CO2 cartridge is
expended and low-pressure gauge reads 0 psi (Figure 14). The pressure on the high-pressure
gauge and the low-pressure gauge should now read 0 psi. If not, carefully bleed pressure until
both gauges read 0 psi, then remove regulators.

23. Remove cell from heating jacket and place in sink. Carefully open valve C and bleed pressure
trapped in the cell. Now, open valve B. All pressure should now be released ( Figure 14).

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Figure 13
Valve Positions to Bleed Pressure

Figure 14
Removing Top and Bottom Pressure Regulators after Bleed Down

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24. Remove Allen screws, being careful to point the top assembly away from your body in case any
pressure may be trapped (Figure 15).

Note: If Allen Screws are tight, DO NOT attempt to remove them because the cell may contain
trapped pressure! This requires special procedures to unplug valves C and B.

Figure 15
Opening the Cell Body

25. Open cell and carefully remove filter paper and cake from screen, being careful not to disturb the
filter cake. Wash excess mud from cake with a small, gentle stream of water.

26. Measure and report thickness of filter cake to nearest 1/32 of an inch. Describe condition of the
cake.

27. Discard the mud. Clean the cell. Cleaning includes removal of valves B and C to prevent mud from
drying in the cell assembly, which could cause valves to plug in future tests.

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Retort -Water, Oil and Solids

Accurate measurement of water, oil and solids content provides fundamental information for control
of mud properties and is essential for evaluating solids control equipment.

The volume percent of liquid phase (water and oil) are measured by heating a known volume of whole
mud in a retort unit. The liquid is evaporated from the mud, vapor is condensed and measured as oil
and fresh water in a graduated glass tube. Suspended solids are calculated by difference of liquid col-
lected subtracted from whole mud volume (retort cup volume).

Retort Test Procedure

Step

1. Clean and dry the retort assembly and condenser. Condenser passage should be cleaned using a
pipe cleaner.

2. Mix the mud sample thoroughly to ensure homogeneity, being careful not to entrain any air, and
that no solids remain on the bottom of container. Air or gas entrapment will cause erroneously high
retort solids due to reduced mud sample volume.

3. Use a clean syringe to obtain a sample of the mud to be tested.

4. Fill retort cup slowly to avoid air entrapment. Lightly tap side of cup to expel air. Place lid on the
cup. Rotate lid to obtain a proper fit. Be sure a small excess of mud flows out of the hole in the lid.
Wipe off any excess mud without wicking any of the sample from inside the cup. Wipe the cup
clean with towel.

5. Pack retort body with steel wool.

6. Apply Never-Seez to threads of retort cup. With lid in place, hand tighten retort cup onto retort
body (Figure 16).

7. Apply Never-Seez to threads on retort stem and attach the condenser.

8. Place the retort assembly inside the heating jacket and close the lid.

9. Place the clean, dry, liquid receiver below the condenser discharge tube. The length of the receiver
may require that it be angled out from the retort and supported off the edge of the work table.

10. Plug cord into 110-volt outlet. Allow the retort to run for a minimum of 45 minutes.

Note: If mud boils over into the receiver, the test must be rerun. Pack the retort with a larger
amount of steel wool and repeat the test.

11. Allow the receiver to cool. Read and record: (1) total liquid volume, (2) oil volume, and (3) water
volume in the receiver.

12. Unplug retort and allow to cool. Disassemble and clean the retort assembly and condenser.

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Figure 16
Retort Instrument

13. Calculate volume percent water (VW), volume percent oil (VO), and volume percent retort solids
(VS), as follows:

100 ( volume of oil, cm 3 )

V O = --------------------------------------------------------------------
V RC
100 ( volume of water, cm 3 )
V W = -----------------------------------------------------------------------------
V RC
100 – ( V W + V O )
V S = -------------------------------------------
-
V RC
V RC = Volume of the retort cup

(See Retort Cup Verification Procedure)

Retort Cup Verification Procedure

Step

1. Allow retort cup, lid and distilled water to reach ambient temperature. Record the temperature.

2. Place the clean, empty retort cup and lid on a balance (precision of 0.01 g) and tare to zero.

3. Fill retort cup with distilled water. Place lid on the cup. Rotate lid to obtain proper fit. Be sure a
small excess of water flows out of hole in lid. Wipe excess water from lid; avoid wicking out water.

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4. Place filled retort cup and lid on the previously tared balance. Read and record weight of water, to
0.01 g.

5. Calculate the retort cup volume, VRC, using density of water at measured temperature from Table 1
as follows:

Weight of water, g
V RC = --------------------------------------------------------------------
-
Density of water , g/cm 3

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Table 1
Density of Water
°F °C Density, g/cm3
59 15 0.9991
59.9 15.5 0.9991
60.8 16 0.9990
61.7 16.5 0.9990
62.6 17 0.9989
63.5 17.5 0.9987
64.4 18 0.9986
65.3 18.5 0.9985
66.2 19 0.9984
67.1 19.5 0.9983
68 20 0.9982
68.9 20.5 0.9981
69.8 21 0.9980
70.7 21.5 0.9979
71.6 22 0.9977
72.5 22.5 0.9976
73.4 23 0.9975
74.3 23.5 0.9974
75.2 24 0.9973
76.1 24.5 0.9971
77 25 0.9970
77.9 25.5 0.9969
78.8 26 0.9968
79.7 26.5 0.9966
80.6 27 0.9965
81.5 27.5 0.9964
82.4 28 0.9962
83.3 28.5 0.9961
84.2 29 0.9959
85.1 29.5 0.9958
86 30 0.9956
86.9 30.5 0.9955
87.8 31 0.9953
88.7 31.5 0.9952
89.6 32 0.9950
90.5 32.5 0.9949
91.4 33 0.9947
92.3 33.5 0.9945
93.2 34 0.9944
94.1 34.5 0.9942
95 35 0.9940

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Sand Content
This simple test is used to determine the volume percent sand-sized particles in a mud. The informa-
tion is used to make adjustments in solids control equipment. Sand causes excessive wear on mixing
equipment, drill string, and on pump parts.

The sand content in a mud system is estimated by wet screen analysis using a 200-mesh (74-micron)
screen. It should be recognized that it is a size-classification of particles and other products, such as
lost circulation materials (LCM), lignite, coarsely-ground barite, etc. will also show up as sand-sized
particles. The presence of these solids, especially LCM, should be noted and quantified if sufficient
volume is present (Figure 17).

Figure 17
Sand Content Equipment

Step

1. Fill glass measure tube to “mud” line with mud. Add water to next scribed mark. Place thumb over
mouth of tube and shake vigorously.

2. Pour mixture onto the clean screen. Add more water to tube and shake. Pour onto screen. Discard
liquid that passes through the screen.

3. Repeat Step 2 until wash water is clean. Then wash sand retained on screen in order to free any
adhering mud.

4. Place funnel on top of screen assembly. Slowly invert assembly and insert tip of funnel into glass
tube. Wash sand back into tube with a fine spray of water or a wash bottle.

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5. Allow sand to settle. Read and record volume percent sand from graduations on the glass measur-
ing tube.

Methylene Blue Capacity

The methylene blue capacity test indicates the concentration of reactive clays present in a drilling
fluid. Reactive clays are commercial bentonite and formation solids such as shales.

Methylene blue dye is added to a sample of whole mud until all reactive sites have adsorbed the dye. A
faint blue/turquoise halo will form around the drop of solids when there is an excess of dye. Drilling
muds frequently contain other materials that adsorb methylene blue. Treatment with hydrogen peroxide
is intended to remove the effects of organic materials such as CMC, polyacrylates, lignosulfonates,
and lignites. Commercial clays such as bentonite and formation solids such as shales adsorb methyl-
ene blue and contribute to the methylene blue capacity of the mud. A variation of the cation exchange
capacity test can be used to determine the reactivity of shales and clays to allow better determination
of the true bentonite concentration in the fluid (Figure 18).

Figure 18
Methylene Blue Test Set-Up

Step

1. If the mud to be tested contains air, stir slowly for 2-3 minutes to release entrapped air.

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2. Use a 2.5 or 3.0-cm3 syringe to measure exactly 2.0 cm3 of drilling fluid.

3. To the Erlenmeyer flask, add 10 cm3 water and 2 cm3 of mud.

4. Next, add 15 cm3 of 3% hydrogen peroxide to the flask. Then, add 0.5 cm3 of 5N sulfuric acid.

5. Gently boil the suspension for 10 minutes on the hot plate.

6. After boiling, remove flask from hot plate and bring the total suspension volume in the Erlenmeyer
flask to 50 cm3 with distilled water. Allow to cool before proceeding to the next step.

7. With a 1-cm3 pipette, add methylene blue to the flask in 0.5-cm3 increments. If the approximate
amount of methylene blue is known from prior testing, larger increments can be added at the
beginning of this titration.) After each addition of methylene blue solution, swirl the contents of flask
for 30 seconds. While the solids are still suspended, remove a drop of liquid on the end of a glass
rod. Place the drop onto a Whatman #1 filter paper. Observe the liquid that wicks out from around
the solids on the paper. The solids will be blue. The liquid will become blue (and form a halo) when
the initial endpoint of the methylene blue titration is reached. (This initial endpoint means that the
active solids are almost saturated with the blue dye, but perhaps not all.)

8. To find the final endpoint, after detecting the initial endpoint, swirl the flask for 2 minutes and place
another drop on a clean area of the filter paper. If the blue ring (or halo) is again evident, the final
endpoint has been reached. If the blue ring is not evident, continue as before adding 0.5-cm3
increments of methylene blue solution - until the blue ring is present after 2 minutes of swirling the
flask.

9. The methylene blue test results are reported as methylene blue capacity (MBC) or as lb/bbl bento-
nite equivalent as in equations (a) and (b) below:

a. MBC = cm3 methylene blue solution/cm3 mud sample

b. lb/bbl bentonite equivalent = 5 (MBC)

pH

Drilling fluid pH measurements and pH adjustments are fundamental to drilling fluid control
because clay interactions, solubility of additives, and contaminant removal are all pH-dependent.

The recommended method for pH measurement is with a pH meter. A portable pH meter (Figure 19 )
consists of a pH probe and an electronic voltage meter. The probe contains:

• glass electrode
• standard reference electrode
• temperature sensor (optional)

Step

1. Measurement consists of: (1) calibration of meter, (2) pH measurement of sample, and
(3) cleaning and storing the probe.

2. Remove end-cap and rinse probe with distilled water. Blot dry.

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Figure 19
pH Meter

3. Allow sample to come to temperature of the buffers and the probe, preferably 70-80°F (20-28°C).

4. Measure temperature of pH7 buffer solution. Place probe into pH7 buffer solution and turn on
meter. Wait for reading to stabilize.

5. Set temperature knob to the temperature of the pH7 buffer solution. Adjust meter calibration knob
to display the temperature-corrected pH. Buffer bottle will list the correct pH value for various tem-
peratures. Rinse electrode with distilled water and blot dry.

6. Repeat Steps 4 and 5 using either pH4 or pH10 buffer. Choose the buffer closest to sample pH
(usually pH10 for muds). If meter does not display correct buffer pH value, adjust calibration knob
to obtain correct pH reading. Rinse electrode with distilled water and blot dry. Place probe back
into pH7 buffer solution and recheck pH. If displayed pH value is the same as previously read in
Step 5, use the slope adjustment screw located at rear of meter to set the correct pH reading.
Then, repeat Step 6 until meter reads correct buffer values.

7. After meter is calibrated with the two buffers, rinse the probe and blot dry. Place probe in sample
and gently stir. Allow reading to stabilize.

8. Record sample temperature in °F or °C. Record the sample’s pH to nearest 0.1.

9. Unplug the meter. Clean probe with distilled water. Saturate the cotton in end cap with pH4 buffer.
Place cap on probe.

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Alkalinity and Lime Content

Alkalinity measurements are used to determine the buffering capacity of a drilling fluid (capacity to
neutralize acidic components or contaminants). From the alkalinity measurements (PM,PF,MF), concen-
tration of hydroxyl (OH-), carbonate (CO3=) and bicarbonate (HCO3-) ions can be estimated. Knowl-
edge of mud and filtrate alkalinities is important to ensure proper mud chemistry control of a drilling
fluid. Hydroxyl alkalinity is necessary for solubilizing some products such as the lignite-based addi-
tives. On the other hand, carbonate and bicarbonate alkalinities adversely affect performance of
clay-based muds.

Table 2
Mud Alkalinity Filtrate Alkalinity
Chemical Tests PM PF (Column 1) MF (Column 2)

Sample 1 cm 3 mud 1 cm3 filtrate con’t from Column 1

Deionized Water 25-50 cm 3 None None

Buffer None None None

4-5 drops 2-3 drops 2-3 drops Methyl Orange

Color Indicator
Phenolphthalein Phenolphthalein
0.02N (N/50) 0.02N (N/50) 0.02N (N/50)
Titrant
H2SO4 (Sulfuric Acid) H2SO 4 (Sulfuric Acid) H2SO4 (Sulfuric Acid)
Pink to Original Mud Pink to Original Mud Yellow to Pink
Color Change
Color Color

cm 3 of 0.02N H SO cm 3 of 0.02N H SO cm 3 of 0.02N H SO

2 4 2 4 2 4
------------------------------------------------------------ ------------------------------------------------------------ ------------------------------------------------------------
cm 3 of mud cm 3 of filtrate cm 3 of filtrate
Record
+
cm 3 of H SO for P
2 4 F
Note Proceed to Column 2

Mud Alkalinity (PM)

Whole mud (liquid + solids) alkalinity is used to estimate the quantity of undissolved lime, which is
used in controlling lime muds and in treating out cement.

Step

1. Measure 1.0 cm3 of mud into a titration vessel using a 2.5 or 3.0-cm3 syringe.

2. Add 50 cm3 of distilled water to the mud sample and stir with stirring rod.

3. Add 5 drops of phenolphthalein indicator solution. A pink color will appear if alkalinity is present.

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4. While stirring, rapidly titrate with 0.02 normal (N/50) sulfuric acid until the pink color disappears.

Note: If endpoint color change is masked, a pH meter can be used to determine when the end-
point of pH8.3 is reached.

5. Report the phenolphthalein alkalinity of the mud, PM, as the number of cm3 of 0.02 normal (N/50)
acid required per cm3 of mud.

Filtrate Alkalinity (PF)

Filtrate (liquid only) PF alkalinity can indicate presence of hydroxyl and carbonate ions in most mud
systems.

Step

1. Measure 1 cm3 of LPLT (Sec. Low-Temperature/Low-Pressure Filtration) filtrate into titration vessel
using a 2.5- or 3.0-cm3 syringe.

2. Add 3 drops of phenolphthalein indicator solution.

3. If indicator turns pink, titrate (drop by drop) with 0.02 normal (N/50) sulfuric acid until the pink color
just disappears.

4. Report the phenolphthalein alkalinity of the filtrate, PF, as the number of cm3 of 0.02 normal acid
require per cm3 of filtrate.

Note: If the indicator color change is masked because of a dark-colored filtrate, the endpoint can
be determined using a pH meter. The endpoint is recorded as the cm 3 of sulfuric acid
required to reduce the filtrate sample pH to 8.3.

Filtrate Alkalinity (MF)

Filtrate (liquid only) MF alkalinity can indicate presence of carbonate ions and can be roughly
related with GGT carbonates.

Step

1. To the same sample which has just been titrated to the PF endpoint, add 3 drops of methyl orange
indicator solution.

2. Titrate with 0.02 normal (N/50) sulfuric acid (drop by drop) while stirring until the indicator changes
from yellow to pink.

3. Report the methyl orange alkalinity (M F) as the total cm3 of 0.02 normal acid per cm3 of filtrate
required to reach the methyl orange endpoint. The MF is recorded as the total volume of acid

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require per cm3 of filtrate. (The total volume includes the cm3 of acid in the PF titration plus the cm3
of acid in the MF titration.)

Note: The endpoint can be determined using a pH meter. The endpoint is recorded as the total
volume of acid required to reduce the filtrate sample pH to 4.3

Estimated concentrations of hydroxyl, carbonate and bicarbonate ions can be determined using
Table 3 below.

Table 3
Ionic Relationships with Alkalinity Titrations
Estimated Concentrations, mg/L

OH - CO3= HCO3-
(Hydroxyls) (Carbonates) (Bicarbonates)
PF = O 0 0 1220 (MF)
2PF < MF 0 1200 (PF) 1220 (MF - 2PF)
2PF = MF 0 1200 (PF) 0
2PF > MF 340 (2PF - MF) 1200 (MF - PF) 0
PF = MF 340 (MF) 0
Note: These equations are valid for very simple filtrates, but become less
valid as the filtrates become more complex with soluble lignite, ligno-
sulfonates, acetates, etc.

Lime Content
Step

1. Determine the PF and PM alkalinities of the mud.

2. Determine the volume fraction of water in the mud, FW, from the retort as follows:

Volume percent water

F W = -----------------------------------------------------------------
100

3. Calculate and report the lb/bbl lime content in the mud using the following equation:

Lime, lb /bbl = 0.26 [ P M – ( F W ) ( P F ) ]

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Chloride

The chloride ion content is a useful indicator of drilling through salt stringers, taking saltwater flows
and for checking the quality of make-up water.

Chloride ion (Cl-) analysis is a titration of the filtrate sample using silver (Ag+) ion to reach an
orange-red endpoint of silver chromate from the potassium chromate indicator. Being able to see this
endpoint is critical. Therefore, technique will depend on the color of the filtrate.

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Table 4
Chloride Titration Chart

Chlorides (CI -) - Light-Colored Filtrates

Chemical Tests Column 1 Column 2
Sample 3 con’t from Col. 1
1 cm filtrate
Deionized Water None 25-50 cm3
Buffer None None

Color Indicator 2-3 drops 8-10 drops

Phenolphthalein Potassium Chromate

Titrate With: 0.02 (N/50) 0.028N AgNO3

(Titrant) H2SO4 or 0.282N AgNO3
(sulfuric acid) *(silver nitrate)
Color Change Pink to original Filtrate Yellow to Orange-Red
color

Record None
( cm 3 0.0282N AgNO 3 ) ( 1000 )
---------------------------------------------------------------------------------
cm 3 Filtrate -OR-

( cm 3 0.282N AgNO 3 ) ( 10, 000 )

------------------------------------------------------------------------------------
cm 3 Filtrate

Note: Proceed to Col. 2 *Chlorides: 10,000 mg/L

If < use: 0.0282N AgNO3
If > use: 0.282N AgNO3

Lightly-Colored Filtrates [Table 4]

Step

1. Measure 1 cm3 filtrate into the titration vessel.

2. Add 2-3 drops phenolphthalein indicator solution.

3. If indicator turns pink, stir sample with glass stirring rod. While stirring, add 0.02N (N/50) sulfuric
acid (drop by drop) until the color disappears.

4. Add 50 cm3 deionized water and 10 drops of potassium chromate solution.

5. Stir continuously while adding silver nitrate solution (Use 0.0282N for chlorides <10,000 mg/L and
0.282N for chlorides >10,000 mg/L.) from pipette until the color changes from yellow to orange-red
and persists for 30 seconds.

6. Record the number of cm3 of silver nitrate solution required to reach the endpoint.

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7. Calculate and report the chloride ion concentration of filtrate, mg/L, as follows:

For Cl- <10,000 mg/L:

( cm 3 of 0.0282N AgNO 3 ) ( 1000 )

Chloride, mg/L = ----------------------------------------------------------------------------------------
-
cm 3 of filtrate

For Cl- >10,000 mg/L:

( cm 3 of 0.282N AgNO 3 ) ( 10, 000 )

Chloride, mg/L = -------------------------------------------------------------------------------------------
-
cm 3 of filtrate

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Table 5
Chloride Titration Chart

Chlorides (CI-) - Dark-Colored Filtrates

Chemical Tests Column 1 Column 2
Sample 3 con’t from Col. 1
1 cm filtrate
Deionized Water None 25-50 cm3
Buffer None 1 g CaCO3
(calcium carbonate)
Color Indicator 2-3 drops 5-10 drops
Phenolphthalein Potassium Chromate

Titrate With: 0.02 (N/50) 0.028N AgNO3

(Titrant) H2SO4 or 0.282N AgNO3
(sulfuric acid) *(silver nitrate)
Color Change Pink to original Filtrate Yellow to Orange-Red
color

Record None
( cm 3 0.0282N AgNO 3 ) ( 1000 )
---------------------------------------------------------------------------------
cm 3 Filtrate -OR-

( cm 3 0.282N AgNO 3 ) ( 10, 000 )

------------------------------------------------------------------------------------
cm 3 Filtrate

Note: Proceed to Col. 2 *Chlorides: 10,000 mg/L

If < use: 0.0282N AgNO3
If > use: 0.282N AgNO3

Dark-Colored Filtrates [Table 5]

Step

1. Measure 1 cm3 filtrate into the titration vessel.

2. Add 2-3 drops phenolphthalein indicator solution. If solution is too dark to observe color, add 2 cm3
of 0.02N (N/50) sulfuric acid and stir.

3. To this solution add 1 g calcium carbonate and stir. While stirring add 50 cm3 deionized water and
10 drops of potassium chromate solution

4. Continue to stir. Add silver nitrate solution (Use 0.0282N for chlorides <10,000 mg/L, and 0.282N
for chlorides >10,000 mg/L.) from pipette until the color changes from yellow to orange-red and
persists for 30 seconds.

5. Record the number of cm3 of silver nitrate solution required to reach the endpoint.

6. Report the chloride ion concentration of filtrate in mg/L as follows:

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For Cl- <10,000 mg/L:

( cm 3 of 0.0282N AgNO 3 ) ( 1000 )

Chloride, mg/L = ----------------------------------------------------------------------------------------
-
cm 3 of filtrate

For Cl- >10,000 mg/L:

( cm 3 of 0.282N AgNO 3 ) ( 10, 000 )

Chloride, mg/L = -------------------------------------------------------------------------------------------
-
cm 3 of filtrate

Total Hardness [Table 6]

The hardness of water or mud filtrate is due primarily to the presence of calcium (Ca++) and mag-
nesium (Mg++) ions. The harder the water, the more difficult for many chemicals to function, partic-
ularly bentonite clay. Also, hardness decreases efficiency of most polymers.

Hardness analysis is a titration of divalent cations in a filtrate using EDTA reagent with an indicator that
changes from wine-red to blue at the endpoint. The endpoint will be gray-blue in dark-colored filtrates.

Step

1. Add 50 cm3 deionized water to titration vessel; then, add 2 cm3 (20 drops) of Versenate Hardness
Buffer Solution.

2. Add 10 drops of Versenate Hardness Indicator solution. If calcium and/or magnesium is present in
the deionized water, a wine-red color will develop. If not, the solution will remain blue.

3. While stirring, titrate with EDTA (standard versenate) until solution color changes from wine-red to
blue. DO NOT GO PAST ENDPOINT!

Note: Steps 1-3 have removed the hardness from the deionized water if any was present.

4. Add 1 cm3 of filtrate to the deionized water. If calcium and/or magnesium is present, a wine-red
color will develop. While stirring, titrate (drop by drop) with EDTA until color indicator changes from
wine-red to blue.

5. Note the cm3 of EDTA and calculate hardness, mg/L, as follows:

( cm 3 of EDTA ) ( 400 )
Total hardness, mg/L = --------------------------------------------------------
cm 3 of filtrate

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Table 6
Total Hardness Titration Chart

Total Hardness
Chemical Tests Column 1 Column 2
Sample None 3
1 cm filtrate
Deionized Water 50 cm 3 None

Buffer 2 cm 3 Versenate None

Hardness Buffer
Color Indicator 10 drops Versenate None
Hardness Indicator

Titrate With: EDTA EDTA

(Titrant) (Standard Versenate) (Standard Versenate)

Color Change Wine Red to Blue Wine Red to Blue

Do not go past endpoint!

Record None ( cm 3 of EDTA ) ( 400 )

--------------------------------------------------------
cm 3 Filtrate
Note: Proceed to Col. 2

Calcium and Magnesium [Table 7]

As mentioned under Total Hardness, divalent cations can adversely affect mud properties. Calcium
and Magnesium can affect muds in different ways, therefore, they may need to be analyzed sepa-
rately.

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Calcium analysis is a titration of a filtrate using EDTA reagent, plus a high pH buffer so that the magne-
sium ions are precipitated and only calcium ion is being analyzed.

Table 7
Calcium/Magnesium Hardness Titration Chart
Calcium Magnesium
Chemical Tests Column 1 Column 2 (Mg++)

Sample None 1 cm 3 filtrate None

Deionized Water 50 cm3 None None

Buffer 1 cm3 Versenate None None

Calcium Hardness
Buffer
Color Indicator Pinch of Calver II None None
Indicator Powder

Titrate With: EDTA EDTA None

(Titrant) (Standard Versenate) (Standard Versenate)

Wine Red to Blue Wine Red to Blue None

Color Change
Do not go past end-
point!
Record None Total Hardness -
( cm 3 of EDTA ) ( 400 )
-------------------------------------------------------- Calcium x 243
cm 3 Filtrate

Note: Proceed to Col. 2 This calculation is

based on recorded
results from Total
Hardness and Cal-
cium tests.

Step

1. Add 50 cm3 deionized water to titration vessel, then add 1 cm3 Calcium Hardness Buffer solution.

2. Add a pinch of Calver II indicator powder. If calcium is present, a wine-red color will develop.

3. While stirring, titrate with EDTA (drop by drop) until sample color changes from wine-red to blue.
DO NOT GO PAST ENDPOINT!

4. Add 1 cm3 of filtrate to the deionized water. If calcium is present, a wine-red color will develop.
While stirring, titrate with EDTA (drop by drop) until the color indicator changes from wine-red to
blue.

5. Note the cm3 of EDTA and calculate calcium, mg/L, as follows:

Calcium, mg/L = (-------------------------------------------------------

cm 3 of EDTA ) ( 400 )
-
cm 3 of filtrate

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6. The magnesium ion concentration is determined by difference of the total hardness less the cal-
cium, times a factor of (0.6).

Magnesium, mg/L = [(Total Hardness, mg/L) – (Calcium, mg/L)] (0.6)

Sulfide

If hydrogen sulfide gas (H2S) or soluble sulfides exist in a mud they are very corrosive to the drill
string and may lead to catastrophic pipe failure. H2S, even in low concentrations, presents both
health and environmental hazards. Therefore, the monitoring of soluble sulfides in a mud system is
critical, especially when drilling in areas known to contain H2S. Soluble sulfides can be quantita-
tively determined in a mud filtrate sample using a Garrett Gas Train (GGT).

H2S, when it enters an alkaline mud, immediately ionizes and is neutralized forming sulfide, S=, and
bisulfide, HS- ions. When the mud’s filtrate is put into a GGT and acidified, the original H2S gas is
reformed, liberated and measured by a stain on the Dräger tube in the GGT.

Figure 20
Assembled Garret Gas Train
(Sulfide Analysis)

Step

1. Be sure the Garret Gas Train is clean, dry and on a level surface with the top removed.

2. To Chamber 1, add 20 cm3 of deionized water and 5 drops of defoamer (Figure 21).

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Figure 21
Preparing GGT for Sulfide Analysis

3. To select the correct Dräger tube and sample volume required for the expected sulfide range, use
Table 8 below.

Table 8
Dräger Tube Identification
Sample Volumes and Tube Factors to be
Used for Various Sulfide Ranges

Sulfide Sample Dräger

Range Volume Tube I.D. Tube
(mg/L) (cm3) (See Tube Body) Factor
1.2 - 24 10.0 H2S 100/a 12
1.5 - 48 5.0
4.8 - 96 2.5

60 - 1020 10.0
120 - 2040 5.0 H2S 0.2% A 600*
240 - 4080 2.5

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Note: *Tube Factor 600 is based on a Batch Factor (stenciled on box) of 0.40. For another Batch
Factor (as stenciled on box), a corrected Tube Factor should be calculated:

Correct Tube Factor = ( 600 )  -------------------------------------

Batch Factor
 0.40 

4. Select the correct Dräger tube and sample volume, then carefully break the glass tip off each end
of the Dräger tube (Figure 22).

Figure 22
Breaking Dräger Tube Tip

5. Place the Dräger tube with arrow pointing downward into the bored receptacle. Install flowmeter
tube with the word “Top” in the upward position in Chamber 3. Make sure o-rings seal properly
(Figure 23).

6. Install the top on the gas train and hand-tighten all screws evenly to seal the o-rings.

7. With the regulator backed off (turn regulator handle counterclockwise), connect the carrier gas to
the dispersion tube of Chamber 1 using rubber tubing. Install and puncture a new CO 2 cartridge.
Connect the flexible tubing from Chamber 3 outlet to the Dräger tube ( Figure 24).

8. Adjust the dispersion tube in Chamber 1 to be approximately 1/4 in. above the bottom using the
white adjustment sleeve.

9. To purge air from the GGT, gently flow carrier gas for 30 seconds by turning handle on regulator
clockwise. Check for leaks. Shut off carrier gas (CO 2) by turning regulator handle counterclock-
wise.

10. Collect a sufficient volume of solids-free filtrate obtained from low-pressure/low-temperature filtra-
tion test. If a low concentration of soluble sulfides is anticipated, a larger volume of filtrate will be
needed (as shown in Table 8).

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Figure 23
Dräger Tube Installed in GGT Base

Figure 24
Reassembled GGT with Sulfide Test in Progress

11. Using a hypodermic syringe and needle, inject a measured volume of the solids-free filtrate sam-
ple into Chamber 1 through the rubber septum. Next, with another syringe, slowly inject 10 cm 3 5N
sulfuric acid.

12. Immediately restart the carrier gas flow by turning handle clockwise. The flow rate should be main-
tained between 200-400 cm3/minute (keep ball between two lines on flowmeter). Continue flowing
for a total of 15 minutes. One CO2 cartridge should provide 15-20 minutes of flow at this rate.

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13. Observe changes in appearance of the Dräger tube. Note and record the maximum darkened
length (in units marked on the tube) before the stain front starts to smear.

Note: If sulfites are present in the high-range Dräger tube, an orange color (caused by SO2 may
appear ahead of the black front. This orange region should be ignored. Record only the
darkened length.

Note: For best Dräger tube accuracy, the “Darkened Length” should fill more than half the tube’s
length.

14. Using the measured sample volume, the Dräger tube’s maximum Darkened Length and the Tube
Factor (Table 3), calculate mg/L sulfide as follows:

( Darkened Length* ) ( Tube Factor )

Sulfide, Mg/L = --------------------------------------------------------------------------------------------------
-
Sample Volume, cm 3

*In units marked on the tube

15. To clean the gas train, remove the flexible tubing and remove the top. Take Dräger tube and
flow-meter out of the receptacles and plug the holes with stoppers to keep them dry. Wash the
GGT with a soft brush, warm water and mild detergent. A pipe cleaner may be used to clean the
passages between the chambers. Wash, rinse and blow out the dispersion tube with a dry air.
Rinse the GGT apparatus with deionized water and allow to dry.

A lead-acetate paper disk fitted under the o-ring of Chamber 3 can be substituted for the Dräger
tube in the gas train. The lead-acetate paper will qualitatively show the presence or absence of sul-
fides in the sample. A dark discoloration of the paper is a positive indication of sulfides. After a pos-
itive indication of sulfides, the test should be repeated using a Dräger tube for a quantitative
analysis.

Carbonate/Bicarbonate

Carbonate/bicarbonate contamination is often difficult to detect. It can cause poor filter cake quality
and excessive mud rheology which can lead to problems such as loss of circulation and the sticking
of pipe and logging tools. The Garrett Gas Train is a reliable means of measuring carbonate/bicar-
bonate contamination.

CO2, when it enters an alkaline mud, immediately ionizes and is neutralized forming carbonate (CO3=)
and bicarbonate (HCO3-) ions. When the mud’s filtrate is put into a GGT and acidified, the original CO2
gas is reformed, liberated and measured by the stain on the CO2 Dräger tube (after first being col-
lected in a 1-liter gas bag).

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Step

1. Be sure the Garrett Gas Train is clean, dry and on a level surface, with the top removed.

Note: If CO2 has been used as a carrier gas in the previous test, purge GGT with N2O carrier gas
for at least 1 minute.

2. Add 20 cm3 of deionized water to Chamber 1, then add 5 drops of octanol* defoamer. (*Avoid inha-
lation or skin contact.)

3. Install the top on the gas train and hand-tighten all screws evenly to seal the o-rings.

4. Turn regulator handle counterclockwise to avoid pressurization. Connect flexible tubing to the dis-
persion tube of Chamber 1. Install and puncture N2O cartridge.

5. Adjust the dispersion tube in Chamber 1 to approximately 1/4 in. off bottom using white adjustment
sleeve.

6. See Table 9 for sample volume required for the expected carbonate range and for the Dräger tube
identification.

Table 9
Dräger Tube Identification
Sample Volumes and Tube Factors
to be Used for Various Carbonate Ranges

Carbonate Sample Dräger

Range Volume Tube I.D. Tube
(mg/L) (cm3) (See Tube Body) Factor
25 - 700 10.0
50 - 1500 5.0 CO‘ 0.12%/a 25,000
250 - 7500

7. Gently flow carrier gas for 1 minute by turning handle on regulator clockwise to purge air from the
system. Check for leaks. Shut off carrier gas.

8. Connect the gas bag and stopcock to hand pump. Use a discarded Dräger tube as a connection
and start with an empty gas bag (Figure 25).

9. Fully depress and release hand pump. When the bag is completely empty and free of leaks, the
pump will remain depressed for several minutes. If leakage is detected, first check the pump and
all connections. (See note below.) If the bag is found to leak, discard it.

Note: To check the pump, insert a sealed Dräger tube into pump opening and depress bellows. It
will remain depressed if pump does not leak.

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Figure 25
Checking for Leaks in Gas Bag

10. With the bag fully collapsed, install rubber tubing from the stopcock and bag onto the outlet of
Chamber 3. Close stopcock.

11. Inject a measured volume of solids-free filtrate into Chamber 1 through the rubber septum, using a
hypodermic syringe and needle. Then slowly inject 10 cm3 of 5N sulfuric acid. Gently shake the
gas train to mix acid with sample.

12. Open the stopcock on the gas bag and restart gas flow by turning regulator handle clockwise.
Allow gas bag to gradually fill until the bag is firm to the touch (do not burst it). Try to fill bag over
approximately a 10-minute interval. Shut off flow (turn handle counterclockwise) and close the
stopcock.

13. Carefully break the tip off each end of the Dräger tube.

Figure 26
GGT with Gas Bag in Place for Carbonate Test

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14. Remove the rubber tubing from Chamber 3 outlet and reinstall it onto the upstream end of the
Dräger tube. Attach hand pump to downstream end of the Dräger tube.

15. Open the stopcock on the bag. With steady hand pressure, fully depress the hand pump. Allow
pump to suction gas out of the bag and through the Dräger tube. When chain on pump is fully
extended, once again depress the hand pump. Continue this procedure until the bag is empty. Ten
strokes (one liter) should empty the bag. More than ten strokes indicates leakage has occurred
and the test must be repeated.

16. A purple stain on the Dräger tube indicates the presence of CO 2. Record stain length in units
marked on the Dräger tube including the faint blue tinge ahead of the purple stain. Using the mea-
sured Sample Volume, the Dräger tube Stain Length and Tube Factor (25,000) Table 4, calculate
total soluble carbonates in the filtrate as follows:

Carbonate, mg/L = 25 , 000 ( Stain Length )

--------------------------------------------------------------
Sample Volume, cm 3

Note: For best Dräger tube accuracy, the Stain Length should fill more than half the tube length.
Therefore, Sample Volume must be carefully selected.

17. To clean the GGT apparatus, remove the flexible tubing and top. Wash the GGT with a soft brush,
warm water and mild detergent. A pipe cleaner may be used to clean the passages between the
chambers. Wash, rinse and blow out the dispersion tube with a dry gas. Rinse the GGT apparatus
with deionized water and allow to dry. Periodically replace the gas bag to avoid leaks and contami-
nation.

Potassium

Potassium ions in drilling fluids are used to stabilize water sensitive shales. Maintaining proper
potassium concentration is the key to successful use of potassium-based muds.

This test method is used to determine the concentration of potassium ions in mud filtrates at levels
above 3.5 lb/bbl potassium chloride. K+ ion is precipitated as the perchlorate salt. The potassium ion
concentration is determined by measuring the volume of precipitate in a graduated (Kolmer) tube and
reading the concentration of potassium ions from a previously prepared standardization curve.

Equipment

Centrifuge RPM Calibration

For this test a horizontal swing rotor head centrifuge capable of producing 1800 rpm is required. To
obtain a fairly constant 1800 rpm with the manual centrifuge ( Figure 27), determine the number of rev-
olutions of the rotor per turn of the crank by the following procedure:

Step

1. Move the crank very slowly and count the number of revolutions of the rotor head during one turn
of the crank.

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Figure 27
Horizontal-Swing Rotor Head Centrifuge and Kolmer Tube

2. As an example, to obtain 1800 rpm of the head, the crank must be turned 120 times in 1 minute. At
this rate, the handle must be turned 10 times in 5 seconds. By experimentation, this crank rate can
be easily achieved.

Standard Potassium Calibration Curve Procedure

A standard calibration curve is required for each centrifuge and can be prepared using the following
method. A minimum of three points (3.5, 10.5, and 17.5 lb/bbl KCl is required to obtain an accurate
graph (Figure 28).

Table 10
Filtrate Volumes
for Various KCl Concentrations

Concentration Range
Filtrate Volume
KCl (lb/bbl) K+ (mg/L) (cm3)
3.5-18 5,250-27,000 7.0
18-35 27,000-52,500 3.5
35-70 52,500-105,000 2.0
over 70 over 105,000 1.0

Step

1. Take three Kolmer tubes and add to them: 0.5, 1.5, and 2.5 cm3 of standard potassium chloride
solution. Dilute each Kolmer tube to the 7.0-cm 3 mark with deionized water and agitate.

2. Add 3.0 cm3 of sodium perchlorate solution to the tube. (Do Not Agitate!)

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Figure 28
Potassium Standard Example
Calibration Curve

3. Counterbalance the centrifuge tube with another tube of the same weight. Centrifuge at a constant
speed of 1800 rpm for 1 minute.

4. Read the precipitate volume immediately.

5. Plot the volume of precipitate volume immediately.

Test Procedure - Potassium Ion

Step

1. Measure 7.0 cm3 of filtrate into the centrifuge tube.

2. Add 3.0 cm3 of the sodium perchlorate solution. DO NOT AGITATE! If potassium ions are present,
precipitation occurs immediately.

3. Centrifuge at a constant speed of 1800 rpm for 1 minute. Immediately read and note the precipi-
tate volume.

Note: To see if all the potassium ions have been precipitated, add 2 to 3 drops of sodium perchlo-
rate solution to the centrifuge tube. If a white precipitate forms, repeat the test using the
next smallest filtrate volume selected from Table 10.

4. Report the potassium concentration as lb/bbl of KCl. The potassium ion concentration in mg/L can
be approximated by multiplying the lb/bbl value by 1500.

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Oil-Based Drilling Fluids Testing Procedures

Mud Density

Mud Density is used to control subsurface pressures and stabilize the wellbore.

Mud density is commonly measured with a mud balance capable of ±0.1 lb/gal accuracy. A mud bal-
ance calibrated with fresh water at 70° ±5° should give a reading of 8.3 lb/gal.

Step

1. Measure and record the temperature of the sample of mud to be tested.

2. Place the mud balance base on a flat, level surface.

3. Fill the clean, dry, mud balance cup with the sample of mud to be tested. Rotate cap until it is firmly
seated. Ensure that some mud is expelled through the hole in the cap to remove any trapped air or
gas.

4. Place thumb over hole in cap and hold the cap firmly on the cup. Wash or wipe the outside of the
cup, and dry.

5. Place balance arm on the support base and balance it by moving the rider along the graduated
scale until the level bubble is centered under the center line.

6. Read the density (weight) of the mud shown at the left-hand edge of the rider and report to nearest
0.1 lb/gal. Enter result on API Drilling Mud Report as Weight (lb/gal, lb/ft 3) or Specific Gravity.

Marsh Funnel Viscosity

Marsh Funnel viscosity is used to indicate relative mud consistency or thickness.

Marsh Funnel viscosity is the time required (seconds) for a quart of mud to flow through a 2-in. long,
3/16-in. diameter tube at the bottom of the Marsh Funnel. This viscosity measurement is used to peri-
odically report mud consistency. One quart of water should flow through a Marsh Funnel in 26±
0.5 seconds.

Step

1. Hold one finger over the orifice at the tip of the funnel. Pour the mud sample through the funnel
screen until mud reaches the bottom of the screen (1500 cm3). Place viscosity cup beneath funnel
tip. Remove finger and start stop watch.

2. Stop the watch when the mud level reaches the 1 qt mark on the viscosity cup.

3. Record the number of seconds required to outflow 1 qt of mud. Enter on Drilling Mud Report as
Funnel Viscosity (sec/qt) API.

4. Measure and record temperature of mud sample to ±1°F.

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Rheology

Rheological properties measured with a rotational viscometer are commonly used to indicate sol-
ids buildup, flocculation or deflocculation of solids, lifting and suspension capabilities, and to calcu-
late hydraulics of a drilling fluid.

A rotational viscometer is used to measure shear rate/shear stress of a drilling fluid - from which the
Bingham Plastic parameters, PV and YP, are calculated directly. Other rheological models can be
applied using the same data. The instrument is also used to measure thixotropic properties, gel
strengths. The following procedure applies to a Fann Model 35, 6-speed VG Meter.

Plastic Viscosity (PV) and Yield Point (YP)

Step

1. Obtain a sample of the mud to be tested. Record place of sampling. Measurements should be
made with minimum delay.

2. Fill thermal cup approximately 2/3 full with mud sample. Place thermal cup on viscometer stand.
Raise cup and stand until rotary sleeve is immersed to scribe lie on sleeve. Lock into place by turn-
ing locking mechanism (refer to Figure 1).

3. Place thermometer in thermal cup containing sample. Heat or cool sample to desired test temper-
ature of 115° ±2°F.

4. Flip VG meter toggle switch, located on right rear side of VG meter, to high position by pulling for-
ward.

5. Position red knob on top of VG meter to the 600-rpm speed. When the red knob is in the bottom
position and the toggle switch is in the forward (high) position -this is the 600-rpm speed ( refer to
Figure 2).

6. With the sleeve rotating at 600-rpm, wait for dial reading in the top front window of VG meter to sta-
bilize (minimum 10 seconds. Record 600-rpm dial reading.

7. With red knob in bottom position, flip the VG meter toggle switch to low position by pushing the tog-
gle switch away from you. Wait for dial reading to stabilize (minimum 10 seconds). Record 300-rpm
dial reading. [See Step 8 to calculate the Plastic Viscosity and Yield Point].

8. The Plastic Viscosity and Yield Point are calculated from the 600-rpm and 300-rpm dial readings
as follows:

PV,cP =  600-rpm  –  300-rpm 

 dial reading  dial reading

YP,lb/100 ft 2 =  300-rpm  –  Plastic 

 dial reading  Vis cos ity

Gel Strength (10-sec/10-min)

Step

1. With red knob in bottom position, flip toggle switch to 600-rpm position (forward position). Stir mud
sample for 10 seconds.

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2. Position red knob to the 3-rpm speed. When the red knob is in the middle position and the toggle
switch is in low (rear) position - this is the 3-rpm speed. Flip toggle switch to off position. Allow mud
to stand undisturbed for 10 seconds.

3. After 10 seconds, flip toggle switch to low (rear) position and note the maximum dial reading. This
maximum dial deflection is the 10-second (initial) gel strength in lb/100 ft2. Record on the mud
check sheet.

4. Pull toggle switch to high and position red knob to 600-rpm speed. Stir mud for 10 seconds.

5. After 10 seconds, and while mud is still stirring, position red knob to the 3-rpm speed. Flip toggle
switch to off position and allow mud to stand undisturbed for 10 minutes.

6. After 10 minutes, flip toggle switch to low (rear) position and note the maximum dial reading. This
maximum dial deflection is the 10-minute gel strength in lb/100 ft2. Record on the mud check
sheet.

Static Filtration Tests

Control of filtration properties of a drilling fluid can be useful in reducing tight hole conditions and
fluid loss to formations.

Static filtration tests are used to indicate filter cake quality and filtrate volume loss for a drilling mud
under specific testing conditions. Filtration characteristics are affected by the types and quantities of
solids and their physical and chemical interactions. Temperature and pressure further affect these sol-
ids and their interactions.
The following instructions for Low-Pressure/Low-Temperature Filtration and High-Pressure/High-Tem-
perature Filtration will be applicable only to equipment used at DTC’s training lab. To operate any other
units, manufacturer’s instructions should be carefully read before attempting to perform testing.

Low-Temperature/Low-Pressure Filtration
Step

1. Open main air valve by turning handle (located on lab bench) counter clockwise. Adjust regulator
to read 100 psi.

2. Be sure cell components, especially the screen, are clean and dry. Check gaskets and discard any
that are worn or distorted.

3. Assemble filtration cell (as illustrated in Figure 3). Lock cell bottom into position by turning cell
body until peg locks into J slot.

4. Pour mud sample to within 1/2 in. of top of cell. Place cell onto filter press rack.

5. Position cell lid onto top of cell body. To seal, turn filter press handle clockwise until hand-tight.

6. Place a clean, dry graduated cylinder under the drain tube of the filtration cell assembly.

7. Close bleeder valve. Maintain in the closed position while test is running (refer to Figure 4).

8. Set interval timer for 30 minutes. Open valve located on filter press manifold by turning black knob
counterclockwise. Pull timer arm down and begin timing immediately.

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9. At the end of 30 minutes, remove graduated cylinder. Measure and record filtrate volume collected.
Volume is measured in cm3/30 minutes. Close valve by turning black knob clockwise. Open
bleeder valve and release trapped line pressure.

10. Turn filter press handle counterclockwise to remove filtration cell assembly from frame. Pour mud
back into viscosity cup, then carefully disassemble mud chamber.

11. Remove filter paper from screen, being careful not to disturb mud cake. Gently wash excess mud
from cake with a stream of water.

12. Measure and report thickness of filter cake to nearest 1/32 of an inch. Describe cake (i.e., soft,
tough, rubbery, firm, etc.).

High-Temperature/High-Pressure Filtration (HTHP)

To operate this or any other unit, manufacturer’s instructions should be carefully read before attempting
to perform testing. Extreme caution should be used in running this test. Equipment should be cleaned
and maintained in good working condition (refer to Figure 5).

Step

1. Plug heating jacket cord into correct voltage for the unit.

2. Place metal thermometer in hole on outside from of heating jacket. Adjust thermostat and preheat
jacket to 10°F above desired test temperature.

3. While jacket is heating, check o-rings (3) on the following components and replace if worn or dis-
torted:

• High-Pressure Regulator

• Lid/Valve

• Cell Body

(Refer to Figures 6, 7, and 8 for details.)

4. Stir mud sample 10 minutes with a high-speed mixer.

5. Close Valve A by turning black knob clockwise.

6. Turn handle counterclockwise on high pressure regulator, then load CO2 cartridge into chamber
(refer to Figure 6).

7. Close valve B and pour stirred mud sample into cell, leaving 1/2 in. from the top lip to allow for
expansion. Position o-ring in groove inside cell body. Place filter paper on top of o-ring (refer to
Figure 7).

8. Open valve C and seat lid/valve assembly. Lubricate threads of allen screws with silicone grease
and tighten (refer to Figure 8).

9. Close valve C low-pressure shut-off valve.

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10. Invert cell. (The lid/valve assembly is now at the bottom.) Carefully, install cell assembly into heat-
ing jacket.

Caution: The Heating Jacket is hot!

Transfer thermometer from the jacket to the thermometer well located on top of HTHP cell body
(refer to Figure 9).

11. Slip high-pressure regulator (0-1500 psi) onto top of valve B and lock into place with steel ring.

12. Slip low-pressure regulator (0-200 psi) on bottom of valve C. Lock into place with steel ring. Be
sure bleeder valve on low-pressure regulator is in the horizontal (closed) position.

13. With valves B and C closed, apply 100 psi to both the high-pressure regulator and the low-pres-
sure regulator by turning regulator handles clockwise.

14. Open valve B. This is done to maintain 100 psi back pressure in the cell body while heating to the
desired temperature. Heating time should not exceed 1 hour (refer to Figure 10).

15. When desired temperature is reached, increase pressure on high-pressure regulator to 600 psi by
turning regulator handle clockwise.

Note: If pressure on low-pressure regulator rises above 100 psi during the test, cautiously reduce
pressure by drawing off a portion of filtrate using valve D located on bottom of filtrate col-
lection chamber.

16. Open valve C. Start timer immediately at this point! Collect filtrate for 30 minutes, maintaining test
temperature within ±5°F (refer to Figure 11).

17. At the end of 30 minutes close valve C. Carefully open valve D and collect filtrate. Leave valve
open until low-pressure gauge reads 0 psi.

18. Note the total volume of filtrate, test temperature and pressure, and cell heat-up time. Because
most HTHP filter presses have a filter area of 3.5 in.2, the filtrate volume collected must be doubled
to correct to API standard 7.1 in.2 Calculate and record the API HTHP filtrate as follows: API HTHP
Filtrate = (2) (cm3 filtrate collected).

19. Unplug unit and allow cell and contents to cool to room temperature before proceeding to disas-
sembly procedure.

Note: CAUTION — Throughout the disassembly procedure, Always assume there could be
trapped high pressure in the HTHP unit.

20. After HTHP cell assembly and contents are cooled to room temperature, proceed with disassem-
bly and cleaning procedure. Valves B and C should already be in the closed positions (refer to
Figure 12).

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21. To bleed pressure from the high-pressure (top) regulator, be sure Valve B is closed. Turn regulator
handle clockwise and carefully open Valve A. Bleed pressure until CO2 cartridge is expended and
high-pressure gauge reads 0 psi (refer to Figure 13).

22. To bleed pressure from the low-pressure (bottom) regulator, be sure that valve C is closed. Turn
regulator handle clockwise and carefully open valve D. Bleed pressure until CO2 cartridge is
expended and low-pressure gauge reads 0 psi (refer to Figure 14). The pressure on the high-pres-
sure gauge and the low-pressure gauge should now read 0 psi. If not, carefully bleed pressure
until both gauges read 0 psi, then remove regulators.

23. Remove cell from heating jacket and place in sink. Carefully open valve C and bleed pressure
trapped in the cell. Now, open valve B. All pressure should now be released ( refer to Figure 14).

24. Remove Allen Screws, being careful to point the top assembly away from your body in case any
pressure may be trapped (refer to Figure 15).

Note: If Allen Screws are tight, DO NOT attempt to remove them because the cell may contain
trapped pressure! This requires special procedures to unplug valves C and B.

25. Open cell and carefully remove filter paper and cake from screen, being careful not to disturb the
filter cake. Wash excess mud from cake with a small, gentle stream of base oil.

26. Measure and report thickness of filter cake to nearest 1/32 of an inch. Describe condition of the
cake.

27. Discard the mud. Clean the cell. Cleaning includes removal of Valves B and C to prevent mud from
drying in the cell assembly, which could cause valves to plug in future tests.

Retort - Water, Oil and Solids

Accurate measurement of water, oil and solids content provides fundamental information for control
of mud properties and is essential for evaluating solids control equipment.

The volume percent of liquid phase (water and oil) are measured by heating a known volume of whole
mud in a retort unit. The liquid is evaporated from the mud, vapor is condensed and measured as oil
and fresh water in a graduated glass tube. Suspended solids are calculated by difference of liquid col-
lected subtracted from whole mud volume (retort cup volume).

Retort Test Procedure

Step

1. Clean and dry the retort assembly and condenser. Condenser passage should be cleaned using a
pipe cleaner.

2. Mix the mud sample thoroughly to ensure homogeneity, being careful not to entrain any air, and
that no solids remain on the bottom of container. Air or gas entrapment will cause erroneously high
retort solids due to reduced mud sample volume.

3. Use a clean syringe to obtain a sample of the mud to be tested.

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4. Fill retort cup slowly to avoid air entrapment. Lightly tap side of cup to expel air. Place lid on the
cup. Rotate lid to obtain a proper fit. Be sure a small excess of mud flows out of the hole in the lid.
Wipe off any excess mud without wicking any of the sample from inside the cup. Wipe the cup
clean with towel.

5. Pack retort body with steel wool.

6. Apply Never-Seez to threads of retort cup. With lid in place, hand tighten retort cup onto retort
body (refer to Figure 16).

7. Apply Never-Seez to threads on retort stem and attach the condenser.

8. Place the retort assembly inside the heating jacket and close the lid.

9. Place the clean, dry, liquid receiver below the condenser discharge tube. The length of the receiver
may require that it be angled out from the retort and supported off the edge of the work table.

10. Plug cord into 110-volt outlet. Allow the retort to run for a minimum of 45 minutes.

Note: If mud boils over into the receiver, the test must be rerun. Pack the retort with a larger
amount of steel wool and repeat the test.

11. Allow the receiver to cool. Read and record: (1) total liquid volume, (2) oil volume, and (3) water
volume in the receiver.

12. Unplug retort and allow to cool. Disassemble and clean the retort assembly and condenser.

13. Calculate volume percent water (VW), volume percent oil (VO), and volume percent retort solids
(VS), as follows:

V O = 100 ( volume of oil, cm 3 )

--------------------------------------------------------------------
V RC
100 ( volume of water, cm 3 )
V W = -----------------------------------------------------------------------------
V RC
V S = 100 – ( V W + V O )
V RC = Volume of the retort cup

(See Retort Cup Verification Procedure )

Retort Cup Verification Procedure

Step

1. Allow retort cup, lid and distilled water to reach ambient temperature. Record the temperature.

2. Place the clean, empty retort cup and lid on a balance (precision of 0.01 g) and tare to zero.

3. Fill retort cup with distilled water. Place lid on the cup. Rotate lid to obtain proper fit. Be sure a
small excess of water flows out of hole in lid. Wipe excess water from lid; avoid wicking out water.

4. Place filled retort cup and lid on the previously tared balance. Read and record weight of water to
0.01 g.

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5. Calculate the retort cup Volume, VRC, using density of water at measured temperature from
Table 1 as follows:

Weight of water, g
V RC = ---------------------------------------------------------------------
Density of water , g/cm 3

Whole Mud Alkalinity (VSA) and Lime Content (LimeOM)

The alkalinity of an oil mud is used to calculate the pounds per barrel of excess lime. Excess alka-
line materials, such as lime, help stabilize the emulsion and also neutralize acid gases such as
hydrogen sulfide and carbon dioxide.

To measure oil mud alkalinity, the emulsion is broken with a solvent and diluted with water and then
titrated with 0.1N H2SO4 to the phenolphthalein endpoint.

Step

1. Add 100 cm3 of 50-50 xylene/isopropanol solvent to a 1000-cm 3 Erlenmeyer flask.

2. Fill a 5-cm3 syringe past the 3-cm3 mark with mud to be tested.

3. Displace 2 cm3 mud into the flask; swirl until the mixture is homogenous.

4. Add 200 cm3 of de-ionized water to the mixture; then add 15 drops of phenolphthalein indicator
solution.

5. While stirring rapidly with a magnetic stirrer, slowly titrate with 0.1N sulfuric acid until pink color dis-
appears; continue stirring. If no pink color reappears within 1 minute, stop stirring.

Note: It may be necessary to stop the stirring to allow the phases to separate in order to see the
endpoint.

6. Let sample stand 5 minutes; IF NO PINK COLOR REAPPEARS, the endpoint has been reached.
IF A PINK COLOR RETURNS, titrate a second time with sulfuric acid. If pink color returns again,
titrate a third time. If, after the third titration a pink color returns, call this the endpoint anyway.
Record the cm3 of 0.1N sulfuric acid required to reach endpoint. Save the mixture for Whole Mud
Chloride test.

7. Calculate Whole Mud Alkalinity (VSA); then, calculate Lime Content (LimeOM) as follows:

cm 3 0.1N Sulfuric Acid

V SA = -----------------------------------------------------------------
cm 3 of mud
Lime O M , lb/bbl = ( V SA ) ( 1.295 )

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Whole Mud Chloride (ClOM)

The chlorides in an oil mud (ClOM) are used with other data to calculate the salinity of the aqueous
phase and from there, to calculate solids content.

Step

1. Using the same sample from the whole mud alkalinity test, ensure that the mixture is acidic (below
pH 7.0) by adding 1-2 drops of 0.1N sulfuric acid.

2. Add 10-15 drops of potassium chromate indicator solution. While stirring rapidly with a magnetic
stirrer, slowly titrate with 0.282N silver nitrate until a salmon pink color remains stable for at least
1 minute. Record cm3 of 0.282N silver nitrate per cm3 of sample (2 cm3) required to reach end-
point. (This is VSN on the Mud Report.)

Note: Additional potassium chromate indicator solution may be required during titration process
and it may be necessary to stop the stirring of the mixture and allow separation of the two
phases to occur to see the color of the aqueous phase.

3. Calculate Whole Mud Chlorides (ClOM) as follows:

3 of 0.282N Silver Nitrate

V SN = cm
---------------------------------------------------------------------------------
cm 3 of mud
CI OM , mg/L = ( V SN ) ( 10, 000 )

Whole Mud Calcium (CaOM)

Calcium in an oil mud (CaOM) is used with other data to calculate the calcium chloride and sodium
chloride content aqueous phase salinity in a mixed brine or super-saturated brine phase of oil mud.

To measure oil mud calcium, the emulsion is broken with a solvent and diluted with water and then
titrated with 0.1M EDTA after adding high pH butter and color indicator.

Step

1. Add 100 cm3 of 50-50 xylene/isopropanol solvent to 1000-cm3 Erlenmeyer flask.

2. Fill a 5-cm3 syringe past the 3-cm3 mark with mud to be tested.

3. Displace 2 cm3 mud into the flask. Swirl until the mixture is homogeneous.

4. Add 200 cm3 of deionized water to the mixture and then add 3.0 cm3 1.0 N sodium hydroxide
buffer solution.

5. To the same mixture add 0.1-0.25 g Calver II indicator powder.

6. Stir rapidly with a magnetic stirrer for 2 minutes.

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7. Let sample stand 5 minutes. If a reddish color appears in the aqueous (lower phase), this indicates
that calcium is present.

8. Place flask on magnetic stirrer. While rapidly stirring, slowly titrate with 0.1M EDTA until a distinct
color change from the reddish color to a blue-green endpoint is reached. Record cm3 of EDTA per
cm3 of sample (2 cm3) to reach endpoint. This is Ca OM on the mud report.

9. Calculate Whole Mud Calcium (CaOM) as follows:

cm 3 of 0.1M EDTA
V EDTA = -----------------------------------------------------
cm 3 of Mud
Ca O M , mg/L = ( V EDTA ) ( 4000 )

Electrical Stability (ES)

The relative stability of a water-in-oil emulsion mud is indicated by the breakdown voltage at which
the emulsion becomes conductive.

The ES test utilizes a probe with a pair of electrodes which are placed in the oil mud. A voltage is
applied until the mud conducts a current. The ES value is indicated by a light on the instrument. This
test procedure is for the Fann Model 23C. The 23C will be replaced by the automated, sine-wave Fann
23D model (see Figure 29).

Figure 29
Electrical Stability Meter

Step

1. Place sample which has been screened through a Marsh funnel into a thermal cup. Hand stir with
ES probe for 30 seconds.

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2. Heat sample to 120 ±5°F and record the temperature on the Drilling Mud Report.

3. Set ES meter dial to zero. Immerse probe into mud sample. Ensure that the probe does not touch
the sides or bottom of the thermal cup.

4. Depress the red power button and hold it down during entire test. DO NOT MOVE probe during
measurement.

5. Starting from a zero reading, gradually increase the voltage by turning the knob clockwise at a rate
of 100-200 volts per second until red indicator light illuminates. Note dial reading. Return dial to
zero. Wipe probe and thoroughly clean between the electrode plates with a paper towel. Repeat
test to determine accuracy ±5% variation is satisfactory.

Note: DO NOT USE detergent solutions or aromatic solvents such as xylene to clean the probe
or cable.

6. Electrical stability (ES) in volts is calculated as follows:

ES, volts = (2) (Dial Reading)

Sulfide

When hydrogen sulfide gas (H2S) enters an oil mud it ionizes and slowly reacts with excess lime to
form calcium sulfide salts. These active sulfides are able to revert to H 2S gas, if the oil mud is con-
taminated by acidic water flow or by a high CO 2 influx. Free H2S gas, even in low concentration, or
active sulfide salts in high concentration present both a health and safety hazard on the rig. There-
fore, monitoring active sulfides in an oil mud is critical, especially when drilling in known high H2S
areas. Active sulfides can be quantitatively determined in a whole mud sample, not a filtrate, using
a modified GGT test.

The oil mud sample to analyzed for sulfides is the whole mud, and not the filtrate. The sulfides of inter-
est - that can be dangerous - are the sulfides that result from H 2S reactions with lime plus any unre-
acted H2S. Therefore, it is necessary to analyze both liquid and solid phases of an oil mud. In the GGT
a weak acid, citric acid (2M) with pH1.8, is used to avoid generating spurious sulfides from certain
metal sulfide minerals. Sulfuric acid should not be used for this test as it is a strong acid and will liber-
ate H2S from accessory minerals in barite.

Step

1. Be sure the Garrett Gas Train is clean and dry. Position gas train on magnetic stirrer so that it is
level. (Remove rubber feet off GGT base.) Remove the top of the gas train and insert a
teflon-coated magnetic stir bar to Chamber 1.

2. Arrange the magnetic stirrer and gas train body so that the stir bar will rotate freely and vigorously
agitate the contents of Chamber 1.

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Figure 30
Garret Gas Train

3. With the gas regulator backed off, install and puncture a CO2 cartridge. (Bottled nitrogen (N2) or
helium (He) is preferred.)

Note: CAUTION — DO NOT use air or nitrous oxide (N2O) as a carrier gas.

4. Arrange the plastic injection tube through the rubber septum located on the top of Chamber 1 to
allow the mud sample to be slowly injected to the bottom of Chamber 1 with a hypodermic syringe.

5. Add 20 cm3 of 2M citric acid solution containing the demulsifier. (See note below to prepare citric
acid solution.)

Note: Citric Acid Solution (2 molar) containing Dowell Fluid Services Oil-Mud Demulsifier is pre-
pared by dissolving 420 g reagent-grade citric acid, (C6H8O7 . H2O) into 1000 cm3 de-ion-
ized water. To this citric acid solution, add 200 cm3 of isopropanol and 25 cm3 of Dowell

6. Add 10 drops of octanol* to the contents of Chamber 1. (*Avoid inhalation or skin contact.)

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7. Select the correct Dräger tube and sample volume required for the expected sulfide range (See
Table 9).

Table 11
Dräger Tube Identification
Sample Volumes and Tube Factors
to be Used for Various Sulfide Ranges

Sulfide Sample Dräger

Range Volume Tube I.D. Tube
(mg/L) (cm3) (See Tube Body) Factor
1.2 - 24 10.0 H2S 100/a 12
1.5 - 48 5.0
4.8 - 96 2.5

60 - 1020 10.0
120 - 2040 5.0 H2S 0.2% A 600*
240 - 4080 2.5
*Tube Factor 600 is based on a Batch Factor (stenciled on box) of 0.40.
For another Batch Factor (as stenciled on box), a corrected Tube Factor
should be calculated:
Correct Tube Factor = 600  -------------------------------------
Batch Factor
 0.40 

8. Break the tip off each end of the Dräger tube. Place the Dräger tube with the arrow pointing down-
ward into the bored receptacle. Install flowmeter tube with the word, Top, in the upward position in
Chamber 3. Make sure o-rings seal properly (Figure 31).

9. Install the top on the gas train, and hand tighten all screws evenly to seal the o-rings.

10. With the regulator backed off (turn regulator handle counter-clockwise), connect the carrier gas to
the dispersion tube of Chamber 1 using latex rubber or flexible inert plastic tubing. Do not clamp
tubing. Connect the flexible tubing from Chamber 3 outlet to the Dräger tube.

11. Adjust the dispersion tube in Chamber 1 to clear the stir-bar. Allow clearance of approximately
1/4 in. off the bottom by loosening the white adjustment sleeve.

12. To purge air from the GGT, gently flow carrier gas for 30 seconds by turning handle on regulator
clockwise. Check for leaks. Shut off carrier gas by turning regulator handle counterclockwise.

13. With contents of Chamber 1 rapidly stirring, slowly inject a measured volume of oil mud through
the injection tube using a hypodermic syringe. Keep the injection tube sealed with the syringe dur-
ing the test. A rubber band can be used to hold the syringe plunger in place. Stir at least 5 minutes
or until the sample is well dispersed with no obvious oil drops.

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Figure 31
Flowmeter and Dräger Tube Installed in GGT Base

14. Immediately restart the carrier gas flow by turning the regulator handle clockwise. Adjust the rate
between 200 to 400 ml/min (keep the flowmeter ball between the red lines on the flowmeter). Con-
tinue flowing for a total of 15 minutes.

Note: One CO2 cartridge should provide about 15 to 20 minutes of flow at this rate.

15. Observe changes in the appearance of the Dräger tube. Note and record the maximum darkened
length (in units marked on the tube) before the stain front starts to smear. Continue the gas flow for
a total of at least 15 minutes. With prolonged flow, the stain front may appear as a diffuse, feathery
coloration. In the high-range tube, an orange color may appear ahead of the black front if sulfites,
SO2=, are present in the sample. This orange region should be ignored. Record only the darkened
length.

16. Using the measured Sample Volume, the Dräger tube’s maximum Darkened Length, and the Tube
Factor from Table 9, calculate the active sulfides as H2S in the sample as follows:

( Darkened Length* ) ( Tube Factor )

H 2 S, mg/L = ---------------------------------------------------------------------------------------------------
( Sample Volume, cm 3 )

* In units marked on the tube.

17. To clean the gas train, remove the flexible tubing and remove the top. Take the Dräger tube and
flowmeter out of the receptacles and plug the holes with stoppers to keep them dry. Clean the
chambers with warm water and a mild detergent, using a soft brush. Use a pipe cleaner to clean
the passages between chambers. Wash the dispersion tube and the injection tube with mineral oil,
and then blow out the tube with air of CO 2 gas. Rinse the unit with deionized water, and allow it to
drain dry. If the dispersion tube frit plugs with solids, such as CaCO3 which forms from using CO2
carrier gas, soak the dispersion tube frit in strong acid; rinse thoroughly, and blow it dry with gas.

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Aqueous Phase Activity (AWOM)

An oil-based mud which is used to drill water-sensitive shale sections must contain a large amount
of salt dissolved in its water phase in order to prevent shale hydration and swelling, otherwise insta-
bility of these shales may result. Effective salinity of an oil mud’s water phase can be measured as
activity by measuring the water’s vapor pressure or relative humidity in air. The Activity Test is a
simple test that can be used at the rig and is very helpful in oil mud engineering in cases when the
salts in an oil mud are too complex (mixed salts) to be accurately measured by API titration meth-
ods.

Introduction
The activity test uses an electrohygrometer (relative humidity meter) to measure the amount of water
vapor that exists in air above an oil mud when sealed in a jar at room temperature. Water’s vapor pres-
sure, at a given temperature, depends on the concentration of dissolved salts in the solution. Activity is
also related to the osmotic pressure that a solution can develop across a semi-permeable membrane -
which exists when shales are coated with an oil mud. By keeping salt at a given concentration in the
water phase of an oil mud, the osmotic pressure can be matched with that of the formation so that
water is not adsorbed into the shale. Salt in very high concentration can even draw water out of a
shale, hardening a wellbore and making the shale stronger to allow it to be drilled faster with less mud
weight in some cases. Measuring and controlling salinity of oil mud is a key part of oil mud technology
as applied at the rig site along with other tests and analyses.

Equipment
The following equipment is needed to measure oil mud activity:

1. Electrohygrometer with a moisture detector capable of measuring relative humidity (RH) from 20%
to 100% (see Figure 32).

2. Standard saturated salt solutions, which are used for calibrating the electrohygrometer RH read-
ings into water activity, AWS. Salt solutions are prepared using deionized water and pure salts as
shown in Table 12. These solutions must be saturated, showing undissolved crystals at room tem-
perature. Approximately 40 cm3 of each of the four saturated salt solutions along with salt crystals
are poured into four of the Fleakers (described below).

3. Fleakers (150-cm3 capacity) - A wide-mouthed calibrated container with special rubber cap made
by Dow Corning Glass Co. One of the caps must be bored and the hygrometer probe stuck
through it so that the probe sensor is about 1.5 in. from the bottom when the cap is on tightly
(Figure 1). Six Fleakers are used: one (#1) for drying agent; four (#2-#5) for salt solutions agent;
and, one (#6) for oil mud sample—and for storing probe when not in use.

4. Drying Agent (desiccant) - DrieriteR or anhydrous calcium sulfate, CaSO4, placed into a Fleaker to
approximately 40-cm3 mark.

5. Insulating Cover - such as a Styrofoam jacket, to fit around the Fleaker (to maintain an even tem-
perature).

6. Graph Paper - linear 10 x 10 per in. scale.

7. Thermometer - range 32-220°F.

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Figure 32
Digital Electrohygrometer and Probe in Fleaker

Table 12
Standard Saturated Salt Solutions

Salt Amount in Water Activity Fleaker

Name, Formula g/100 cm3 AWS #
Calcium chloride, CaCl2 100 0.30 2
Calcium nitrate, CaNO3 200 0.51 3
Sodium chloride, NaCl 200 0.75 4
Potassium nitrate, KNO3 200 0.94 5

Procedure
The procedure (as given in API RP 13B-2, Appendix C) is also outlined here.

The electrohygrometer must be frequently calibrated at the start and every few days using the stan-
dard salt solutions. A calibration graph must be prepared each time. The oil mud activity is found by

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measuring its relative humidity and reading AWOM from the calibration graph. (Salt solutions can be
used many times, as long as they are not contaminated or allowed to absorb water from the air.)

Note: CAUTION: DO NOT TOUCH the sensor element on the probe. DO NOT allow salt water or
oil mud to contact the sensor. IF THE SENSOR IS CONTAMINATED, IT MUST BE
REPLACED.

Preparation of Calibration Graph for the Electrohygrometer:

Step

1. Prepare the graph paper with 0 to 100% RH on the vertical axis and 0 to 1.0 AWS on the horizontal
axis. (See sample graph, Figure 33.)

Figure 33
Example - Calibration Graph for Electrohygrometer

2. Dry the probe to < 24% RH by placing it in the air space above the drying agent in Fleaker #1.

3. Place the RH probe in air above the saturated CaCl2 salt solution in Fleaker #2. Place the Fleaker
in the insulation jacket. Wait at least 15 minutes for RH to reach equilibrium. Plot the RH reading
on meter at 0.30 on graph paper.

4. Repeat Step 2, drying the probe.

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5. Place the RH probe in air above the saturated CaNO3 solution in Fleaker #3. After at least
15 minutes, read RH on the meter. Plot this RH reading at 0.51 AWS on graph paper.

6. Repeat Step 2.

7. Place the RH probe in air above the saturated NaCl solution in Fleaker #4. After at least
15 minutes, read RH on meter. Plot this RH reading at 0.75 AWS on graph paper.

8. Repeat Step 2.

9. Place the RH probe in air above the saturated KNO3 solution in Fleaker #5. After at least
15 minutes, read RH on meter. Plot this RH reading at 0.94 AWS on graph paper.

10. Draw the best-fit straight line through the points on the graph. (The line may not fit the 0.94 AWS as
well as it should, but will likely pass through the other three points.)

11. Seal the standard salt solutions tightly and store at room temperature where they won’t be tipped
over.

Testing Oil Mud Sample - It is CRITICAL that the oil mud sample and the testing equipment (probe)
be at the same temperature before starting this procedure. This avoids water condensation on the sen-
sor.

Step

1. To allow the oil mud sample and equipment to reach the same temperature, place the oil mud sam-
ple, empty Fleaker #6 and stopper which holds the hygrometer probe, side-by-side on the test
bench. Measure the mud temperature and air temperature to be sure they are within 5°F of each
other before proceeding to Step 2.

2. Pour approximately 40 cm3 of oil mud into a clean and dry Fleaker #6. Tilt the Fleaker and rotate it
to make a film of oil mud on sides of the Fleaker. (This provides a larger surface area for water
vapor to escape.)

3. Immediately place cap-with-probe onto the Fleaker containing the oil mud sample. Be sure the
insulated jacket is on the Fleaker (Figure 34).

4. Wait at least 30 minutes for water vapor in oil mud to reach equilibrium with air in the Fleaker. Read
the RH on the meter.

5. Using calibration graph, find the Aw that corresponds to the RH meter reading. Record that as
AWOM of oil mud.

Note: Oil-Based Muds in this Manual has more information on the relationship between activity
and oil mud salinity.

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Figure 34
Fleaker Containing Oil Mud Sample and
RH Probe in Air Space Above Mud

Water-Wet Solids

Water wetting of solids in an oil-based mud begins with the failure of mud to flow through fine shale
shaker screens. Continued problems may result from obstruction inside the drill string by water-wet
solids buildup, causing high pump pressure and the eventual need to ream out the pipe. At latter
stages, water wetting is associated with breaking of the oil mud’s emulsion - causing settling of sol-
ids and disastrous failure (flipping) of the mud system.

There are several operational indicators and trends from the mud engineer’s daily mud checks and a
few special tests that can be used to identify water wetting of oil-mud solids before the problem
becomes serious and irreversible.

Causes of Water-Wet Solids

Common causes of water wetting of solids can be anticipated or seen if the drilling supervisor and mud
engineer are aware of potential problems and are communicating. Some common causes are:

1. Influx of water or contamination by water-based mud into the oil mud.

2. Insufficient oil-wetting chemical put into the oil mud over a period of time.

3. Excessive downhole temperature and high drill solids consuming the oil-wetting chemicals.

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4. Drilling highly water soluble salt formations, such as carnalite and bischofite - magnesium chloride
salts.

5. Adding freshly prepared, poorly treated oil mud into the pits and sending it down hole.

6. Excessive additions of solid CaCl 2 to the oil mud, exceeding aqueous phase saturation, thus allow-
ing free CaCl2 crystals to exist in the mud.

Visual Indicators of Water-Wet Solids

Early visual indicators of water-wet solids are fairly subtle, but the intermediate and latter indicators are
clear cut (such as gross settling and flipping of the mud). Visual indicators are:

1. Dull, grainy appearance of the mud, rather than the normally mirror-like surface.

2. Sticky, agglomerated solids blinding the shaker screens.

3. Pump pressure increasing steadily from solids building up inside the drill string, usually the drill
collars.

4. Settling of agglomerated solids despite adequate gel strengths.

Mud Test Indicators of Water-Wet Solids

Other indications of water-wet solids come from monitoring the mud testing that is routinely performed
on oil-based muds. These indicators are:

1. Rheology - Erratic flow properties resulting from solids agglomeration affecting Fann VG meter
readings.

2. Electrical Stability - Steadily decreasing ES voltages with time resulting from water film on solids
causing a weakened emulsion.

3. HTHP Filtration - High and increasing filtrate volumes with water in the filtrate.

4. Mud Chemistry - Changes in salinity and decrease in lime as a result of: (1) drilling salts such as
carnalite and bischofite; (2) excess treatments with calcium chloride; or (3) a water influx.

5. Retort Analysis - Increasing water content as a result of a water flow or rain or water-mud contam-
ination.

Special Tests and Indicators of Water-Wet Solids

These are special tests that the mud engineer can perform at the rig and observations he can make
during testing which can indicate presence of water-wet solids.

1. Sand Content Test - High percentage of sand-sized particles (agglomerated solids) measured by
the Sand Content Test which screens the mud through a 200-mesh screen. The test for oil mud is
performed as is the water-based mud test for Sand Content, except that oil is used to wash the sol-
ids on the screen rather than water. To show that these solids are actually water-wet and are
agglomerated small particles, wash the oil-mud solids with a mixture of 50:50 xylene:isopropanol.
If they disperse into finer size and pass through the 200-mesh screen, then they were agglomer-
ated.

2. Coating Test - Water-wet, oil-mud solids will adhere to a highly water-wet surface such as clean
glass or clean metal. (That is why solids build up and plug the inside of drill collars.) The Coating
Test is performed by filling a round jar about half full of the oil mud to be examined. The mud is

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stirred at moderate speed with a mixer for 30 minutes. Solids are slung against the glass and if
they are water wet some will stick to the jar. The oil mud is poured out and the jar is left to drain.
The jar is examined for a film. If no film exists (at the level of the stirrer blade) then there is no indi-
cation of water wetting problems. If there is a film, it can be judged by its thickness - the thicker and
more opaque the film or coating, the more water wet are the solids. Also, the film will be difficult to
wash or wipe off when solids are strongly water wet.

3. Settling - When solids settle badly in the testing equipment (mud cup, rheometer cup and mud bal-
ance), yet the mud’s gel strength seems adequate to suspend barite, that is an indication of solids
being water wet and agglomerated.

Lime, Solids and Salinity Calculations

This section describes the calculations for oil mud salinity and solids which only the chloride ion
data and which can be used only for oil muds that contain either CaCl2 or NaCl (not both salts
mixed together). In the event that a “mixed salt” type of oil-based mud is to be analyzed, then it is
necessary to perform the analysis for the calcium ion and to perform the calculations found in API
RP 13B-2, Section 7.

The equations used in this procedure can be solved by using a hand calculator, but it is best to use a
PC program. Several of these programs have been written.

Note: Data used in this API method are not compatible with Drilpro computer programs.

Note: Another test that can be related to oil mud salinity is the Aqueous Phase Activity, AWOM, of
oil muds. The relative vapor pressure of water in air above an oil mud is measured by an
electrohygrometer to find AWOM. This procedure is found in API RP 13B-2, Appendix C and
also is outlined in this manual in Section 3.

Total Lime Content (LimeOM)

Information needed:

VSA = cm3 0.1N sulfuric acid/cm3 oil mud sample

LimeOM = 1.295 (VSA) = lb/bbl

Whole Mud Salinities (ClOM, CaCl2OM, NaClOM)

Information needed:

VSN = cm3 0.282N silver nitrate/cm3 oil mud sample

ClOM = 10,000 (VSN) = mg/L

If salt is assumed to be CaCl2, then:

CaCl2OM = 1.57 (ClOM) = mg/L

If salt is assumed to be NaCl, then:

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Nomenclature

Mud density, lb/gal ................................................................................................ MW

Volume acid for alkalinity, cm3 0.1N H2SO4/cm3 mud ........................................... VSA
Volume silver nitrate for chloride, cm3 AgNO3/cm3 mud ....................................... VSN
Whole mud Ca(OH)2 content, lb/bbl...................................................................... LimeOM
Whole mud Cl- ion content, mg/L .......................................................................... ClOM
Whole mud CaCl2 content, mg/L........................................................................... CaCl 2
OM

Whole mud NaCl content, mg/L ............................................................................ NaCl OM

Oil from retort, vol% .............................................................................................. VO
Water from retort, vol% ......................................................................................... VW
Solids Corrected for salinity, vol% ......................................................................... VS
Density of brine, g/cm3 ....................................................................................................ρB
Density, average of solids, g/cm3 ...................................................................................ρAVG
Density of drill solids, g/cm3 ............................................................................................ρLGS
Volume of drill solids, vol%.................................................................................... VLGS
Concentration of drill solids, lb/bbl ........................................................................ MLGS
Density of weight material, g/cm3 ..................................................................................ρHGS
Volume of weight material, vol% ........................................................................... VHGS
Concentration of weight material, lb/bbl ................................................................ MHGS
Density of base oil, g/cm3 ...............................................................................................ρO
Weight percent CaCl2 in brine, wt% ...................................................................... WC
Weight percent NaCl in brine, wt% ....................................................................... WN
Parts per million, g/10 6g........................................................................................ ppm
Milligrams per liter, g/106cm3 ................................................................................ mg/L
Oil-water-ratio, vol%/vol% ..................................................................................... O/W
Oil-brine-ratio, vol%/vol% ...................................................................................... O/B

NaClOM = 1.65 (ClOM) = mg/L

Aqueous Phase Salinity (Weight Percent)

Information needed:
Retort water %, VW

Weight percent, if salt is assumed to be CaCl2:

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100 ( CaCl 2O M )
W C = ---------------------------------------------------------------------
- = wt% CaCl 2
( CaCl 2O M ) + 10, 000 ( V W )

Weight percent, if salt is assumed to NaCl:

100 ( NaClOM )
W N = ------------------------------------------------------------------
- = wt% NaCl
( NaCl O M ) + 10, 000 ( V W )

Aqueous Phase Salinity - Parts per Million

Information needed:
Weight percent CaCl2, W C

CaCl2 = 10,000 (WC) = ppm

Weight percent NaCl, WN

NaCl = 10,000 (WN) = ppm

Aqueous Phase Salinity (Milligram per Liter)

Information needed:
CaCl2 brine density and NaCl brine density (calculated from polynomial for rB [See Oil/Brine Ratio
(O/B).])

CaCl2 = (CaCl2, ppm) (CaCl2 rB) = mg/L

NaCl = (NaCl, ppm) (NaCl rB) = mg/L

Oil/Water Ratio (O/W)

Information needed:
Raw Data from retort: VO, VW

100 ( V O )
Oil % in O/W = ---------------------------
( VO + V W )
100( V W )
Water % in O/W = ---------------------------
( VO + V W )
O/W = Oil %/Water %

Oil/Brine Ratio (O/B)

Information needed: Brine density for calculating VB.
Brine density for NaCl brine only:

ρB = 0.99707 + 0.006504 (WN) + 0.00004395 (WN)2 = g/cm3

Brine density for CaCl2 brine only:

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ρB = 0.99707 + 0.007923 (W C) + 0.00004964 (WC)2 = g/cm3

Note: Density of CaCl2 brines are found in Table 14 and NaCl brines are found in Table 15.

100 ( V W )
V B = ----------------------------------------- = vol%
( ρ B ) ( 100 – W X )

where

W X = W C or W N

100 ( V O )
Oil % in O/B = -------------------------
-
( V O + VB )

100 ( V B )
Brine % in O/B = -------------------------
-
( VO + VB )

O/B = Oil %/Brine %

Solids Content
Information needed:
Mud density, density of high and low gravity solids, water, oil and brine phases.
Corrected Solids Content, VS, vol%:

VS = 100 - (VO + VB)

Average Density Suspended Solids, rAVG, g/cm3

[ 100 ( M w ) ] – [ ( v o ) ( ρ O ) ] – [ ( V S ) ( ρ S ) ( 8.34 ) ]
ρ AVG = ------------------------------------------------------------------------------------------------------------------
8.34 ( V S )

Volume % and Concentration Low-Gravity Solids:

ρ AVG – ρ LG S
V HGS =  ---------------------------------- ( V S ) = vol%
 ρ HGS – ρ LG S

M HGS = 3.5 ( ρ HGS ) ( V LG S ) = lb/bbl

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Examples of Calculations for Oil Mud Analysis

Given Data Used in Examples

EXAMPLE A EXAMPLE B
Information Needed
CaCl2 Mud NaCl Mud
MW, lb/gal 11.0 11.0
VO, vol% 59.5 59.5
VW, vol% 25.0 25.0
VSA, cm3 acid/cm3 mud 2.6 2.0

VSN, cm3 AgNO3/cm3 mud 5.8 4.4

ρB, g/cm3 brine density (Calculated values)

ρHGS, g/cm 3 4.20 4.20

ρLGS, g/cm 3 2.65 2.65

ρO, lb/gal 7.00 7.00
ρW, lb/gal 8.34 8.34

EXAMPLE A - Oil Mud with CaCl2 Aqueous Phase:

Step

1. Total Lime Content (LimeOM)

Information needed:

cm 3 0.1N sulfuricacid
V SA = -------------------------------------------------------------
cm 3 mud
Lime O M = 1.295 ( V SA )
Lime O M = 1.295 ( 2.6 ) = 3.4 lb/bbl Ca ( OH ) 2

2. Whole Mud Salinities (ClOM, CaCl2OM)

Information needed:

cm 3 0.282N silver nitrate

V SN = -----------------------------------------------------------------------
cm 3 oil mud sample

Salt is assumed to be CaCl2, then:

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CI O M = ( 10, 000 ) ( V SN )
CI O M = 10, 000 ( 5.8 ) = 58, 000 mg/L Chloride
CaCl2 = 1.57 ( CI OM )
OM

CaCl2 = 1.57 ( 58, 000 ) = 91, 060 mg/L CaCl2

OM

3. Aqueous Phase Salinity - weight percent

Information needed: Retort water %, VW

Weight %, salt is assumed to be CaCl2:

100 ( 91, 000 )

W C = ------------------------------------------------------------------
- = 26.7 wt% CaCl 2
( 91, 000 ) + 10, 000 ( 25.0 )

4. Aqueous Phase Salinity - parts per Million

Information needed: Weight percent CaCl2, WC

CaCl2 = 10,000 (26.7) = 267,000 ppm

5. Aqueous Phase Salinity - milligram per liter

Information needed: CaCl2 brine density

ρ B = 0.99707 + 0.007923 ( 26.7 ) + 0.00004964 ( 26.7 ) 2

= 1.24 g/cm 3
CaCl2 = ( CaCl2 , ppm ) ( ρ B )
= 266, 000 ( 1.24 ) g/cm 3
= 329, 840 mg/L CaCl 2

6. Oil/Water Ratio - O/W

Information needed: Raw Data from retort, VO, VW

100 ( 59.5 )
Oil % in O/W = ----------------------------- = 70.4
59.5 + 25.0
100 ( 25.0 ) = 29.6
Water % in O/W = ----------------------------
-
59.5 + 25.0
O/W = Oil % Water % = 70/30

7. Oil/Brine Ratio - O/B

Information needed: Corrected Retort Water, VB

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100 ( 25.0 )
V B = -------------------------------------------- = 27.5 vol%
1.24 ( 100 – 26.7 )
100 ( 59.5 ) = 68.4
Oil % in O/B = -----------------------------
59.5 + 27.5
100 ( 27.5 )
Brine % in O/B = ----------------------------- = 31.6
59.5 + 27.5
O/B = 68/32

8. Solids Content

Corrected Solids, VS, vol%:

Information needed: Retort Oil, VO, and brine, VB

VS = 100 - (59.5 + 27.5) = 13.0 vol%

Average Density of Suspended Solids:

Information needed: Mud, Oil and Water Densities and Retort Data

[ 100 ( 11.0 ) ] – [ ( 59.5 ) ( 7.0 ) ] – [ ( 27.4 ) ( 1.24 ) ( 8.34 ) ]

ρ AVG = -------------------------------------------------------------------------------------------------------------------------------------
8.34 ( 13.0 )
= 3.69 g/cm 3

Volume of High-Density (barite) Solids, vol%:

Information needed: Density of high- and low-gravity solids and V S, vol%.

V HGS = (--------------------------------------------------
3.69 – 2.65 ) ( 13.0 ) = 8.6 vol%
-
4.20 – 2.65

Concentration of High-Density Solids, lb/bbl:

MHGS = 3.5 (4.20) (8.6) = 126.4 lb/bbl

Volume of low-density solids, vol%:

VLGS = 13.0 - 8.6 = 4.4 vol%

Concentration of low-density solids, lb/bbl:

MLGS = 3.5 (2.65) (4.4) = 40.8 lb/bbl

Example B — Oil Mud with NaCl Aqueous Phase

1. Total Lime Content - Lime OM

cm 3 0.1N sulfuric acid

Information needed: V SA = ----------------------------------------------------------------
cm 3 mud

LimeO M = 1.295 ( V SA )
LimeO M = 1.295 ( 2.0 ) = 2.6 lb Ca ( OH ) 2 /bbl mud

2. Whole Mud Salinities - ClOM, NaClOM

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cm 3 0.282N silver nitrate

Information needed: V SN = ------------------------------------------------------------------------
cm 3 oil mud sample

CI OM = 10, 000 ( V SN )
CI OM = 10, 000 ( 4.4 ) = 2.6 lb Ca ( OH ) 2 /bbl mud
NaClOM = 1.65 ( 44, 000 ) = 72, 600 mg/L NaCl

3. Aqueous Phase Salinity - Weight Percent

Information needed:Retort Water %, V W

Weight %, salt is assumed to NaCl:

100 ( 72, 600 )

W N = ------------------------------------------------------------------- = 22.5 wt% NaCl
( 72, 600 ) + 10, 000 ( 25.0 )

4. Aqueous Phase Salinity - Parts per Million

Information needed:Weight percent NaCl, WN

NaCl = 10,000 (22.5) = 225,000 ppm

5. Aqueous Phase Salinity - Milligram per Liter

Information needed: NaCl brine density, ρB

ρ B ( NaCl ) = 0.99707 + 0.006504 ( 22.5 ) + 0.00004395 ( 22.5 ) 2

= 1.17 g/cm 3
NaCl, mg/L = ( NaCl, ppm ) ( ρ B )
= 225, 000 ( 1.17 ) = 263, 200 mg/L NaCl

6. Oil/Water Ratio - O/W

Information needed: Raw Data from Retort, VO, VW

Oil % in O/W = 100 ( 59.5 )/ ( 59.5 + 25.0 ) = 70.4

Water % in O/W = 100 ( 25.0 )/ ( 59.5 + 25.0 ) = 29.6
O/W = Oil %/Water % = 70/30

7. Oil/Brine Ratio - O/B

Information needed: Corrected Retort Water, VB

100 ( 25.0 )
V B = -------------------------------------------
- = 27.6 vol%
1.17 ( 100 – 22.5 )
Oil % in O/B = 100 ( 59.5 )/ ( 59.5 + 27.6 ) = 68.3
Brine % in O/B = 100 ( 27.6 )/ ( 59.5 + 27.6 ) = 31.7
O/B = Oil %/Brine % = 68/32

8. Solids Content - Corrected Solids, vol%, VS:

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Information needed: Retort Oil and Brine, vol%.

VS = 100 - (59.5 + 27.6) = 12.9 vol%

Average Density of Suspended Solids:

Information needed: Mud weight, oil and water densities and retort data.

[ 100 ( 11.0 ) ] – [ ( 59.5 ) ( 7.0 ) ] – [ ( 27.6 ) ( 1.17 ) ( 8.34 ) ]

ρ AVG = -------------------------------------------------------------------------------------------------------------------------------------
8.34 ( 12.9 )
= 3.85 g/cm 3

Volume of High-Density Solids (barite), vol%:

Information needed: Density of high- and low-gravity solids and VS.

ρ AVG – ρ L GS
- = vol%
V HGS = ---------------------------------
ρ HGS – ρ LG S

Concentration of high-density solids, lb/bbl:

MHGS = 3.5 (4.20) (10.0) = 147.0 lb/bbl

Volume of low-density solids, vol%:

VLGS = 12.9 - 10.0 = 2.9 vol%

Concentration of low-density solids, lb/bbl:

MLGS = 3.5 (2.65) (2.9) = 26.9 lb/bbl

Table 13
Commonly Used Densities
(at 20°C)

Mud Component Density, g/cm3 Density, lb/gal Density, kg/m3

Fresh Water 0.998 8.33 998
Diesel Oil #2 0.84 7.000 840
Typical Low Viscosity Oil 0.80 6.700 800
Low Density Solids 2.65 22.100 2650
High Density Solids
Barite 4.20 35.000 4200
Hematite 5.05 42.100 5050

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Table 14
Calcium Chloride Brine Table
(Properties at 20°C)

% CaCl2 Chloride Final Water Density Density

WTC mg/L mg/L Volume Activity g/cm3 lb/gal
0 0 0 1.000 1.000 0.998 8.330
2 20,300 12,990 1.004 0.096 1.0166 8.484
4 41,340 26,410 1.008 0.989 1.0334 8.624
6 63,030 40,280 1.013 0.979 1.0505 8.766
8 85,420 54,590 1.018 0.967 1.0678 8.911
10 108,540 69,360 1.024 0.951 1.0854 9.058
12 132,400 84,600 1.030 0.933 1.1033 9.207
14 157,050 100,360 1.037 0.912 1.1218 9.361
16 182,510 116,630 1.044 0.888 1.1407 9.519
18 208,780 133,410 1.051 0.862 1.1599 9.679
20 235,920 150,750 1.060 0.832 1.1796 9.844
22 263,930 168,650 1.069 0.800 1.1997 10.011
24 292,820 187,100 1.078 0.765 1.2201 10.182
26 322,660 206,170 1.089 0.727 1.2410 10.356
28 353,420 225,820 1.100 0.686 1.2622 10.533
30 385,140 246,885 1.113 0.643 1.2838 10.713
32 417,890 267,020 1.126 0.597 1.3059 10.898
34 451,620 288,570 1.141 0.548 1.3283 11.047
36 486,430 310,780 1.156 0.496 1.3512 11.276
38 522,310 333,740 1.173 0.441 1.3745 11.470
40 559,280 357,370 1.192 0.384 1.3982 11.668
Note: The calcium ion concentration can be determined by subtracting the Chloride
ion value from the Calcium Chloride value.

(Ca++, mg/L = CaCl2, mg/L – Cl, mg/L)

*B. R. Staples and R. L. Nuttall, J. Phys. Chem. Ref. Data. 1977, Vol. 6, No. 2,
p. 385-407.

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Table 15
Sodium Chloride Brine Table
(Properties at 20°C)

% NaCl Chloride Final Water Density Density

WTN mg/L mg/L Volume Activity g/cm3 lb/gal
0 0 0 1.000 1.000 0.9980 8.330
2 20,250 12,310 1.006 0.989 1.0143 8.464
4 41,140 24,960 1.013 0.976 1.0286 8.584
6 62,590 37,980 1.020 0.964 1.0431 8.705
8 84,620 51,350 1.028 0.950 1.0578 8.827
10 107,260 60,680 1.036 0.935 1.0726 8.951
12 130,510 79,200 1.045 0.919 1.0876 9.076
14 154,390 93,680 1.054 0.901 1.1028 9.203
16 178,910 108,570 1.065 0.882 1.1182 9.331
18 204,100 123,840 1.076 0.861 1.1339 9.462
20 229,960 139,540 1.087 0.839 1.1498 9.595
22 265,520 155,660 1.099 0.815 1.1660 9.730
24 283,800 172,210 1.113 0.788 1.1825 9.868
26 311,820 189,210 1.127 0.759 1.1993 10.008
Note: The sodium ion concentration can be determined by subtracting the Chloride
ion value from the Sodium Chloride value.

(Na+, mg/L = NaCl, mg/L – Cl, mg/L)

*E. C. W. Clarke and D. N. Grew, J. Phys. Chem. Ref. Data. 1985, Vol. 14,
No. 2, p. 489-610

Permeability Plugging Test (PPT)

Introduction
The Permeability Plugging Test (PPT) Apparatus is a modified HTHP fluid loss cell that is used for esti-
mating static fluid loss under downhole conditions (wellbore temperature and differential pressure).
The filtrate of the drilling fluid can be measured and additives selected which will minimize this filtra-
tion, leading to less chance of differential sticking.

For economic reasons, many wells are currently drilled using fewer casing strings resulting in long
open hole intervals and high differential pressures. Thus, the potential for differential sticking is signifi-
cantly increased, especially when drilling through depleted intervals. To successfully drill these wells,
properly designed muds and accurate pore pressure predictions are essential. The fluid must be not
only inhibitive, but also must deposit a very low permeability filter cake to seal underpressured forma-
tions. The Permeability Plugging Test, which uses disks of selected permeability, measures fluid loss at

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downhole temperature and differential pressure to predict drilling fluid performance under these condi-
tions. Using the PPT, the effects of high differential pressure are readily apparent by measuring: spurt
loss, total fluid loss, and cake thickness. In the PPT these properties are substantially different than
those seen with HTHP fluid loss cells with filter paper.

PPT Principles
In running the PPT test, it is important to remember that the type of mud and the pore size of the disk
used for the test will influence the results. The disks are meant to simulate the porous formations
encountered in drilling. Trends are important to monitor rather than absolute values. Results of prod-
ucts run in different types of mud should not be compared.
The important parameter to consider is the ratio of the size of the particles in the mud and the pore
size in the rock. Generally speaking, when the ratio of the particle size to pore size is less than 1/6,
whole mud will pass through the formation and bridging will not occur. A ratio of 1/2 or greater will form
a filter cake and intermediate values will show invasion with bridging (spur) until the effective bridged
ratio is greater than 1/2 and the filter cake forms. No leakoff control can be obtained until a filter cake is
formed.

When the mud contains very fine particles relative to the pore size, i.e., the ratio is less than 1/6, SCM
is added as a bridging agent to allow a filter cake to form. SCM will bridge the pores until the effective
pore size is reduced and filter cake can form. The SCM may also effect the quality of the filter cake
such that both loss of whole mud and normal fluid loss (filtrate) are reduced. A given SCM’s perfor-
mance will be related to the core pore size that it is tested against. The performance of a SCM will also
be a function of the mud type.

The deposition of a filter cake and bridging of pores is covered in filtration theory. The equations cover-
ing filtration have been known for several years. The basic form presented here for filtration with inva-
sion comes from Barkman and Davidson:1

S2
V = S t + V B – -----------
2Q B

where

V = cumulative throughput volume

S = slope of cumulative volume vs. square root of time

t = total time of filtration

VB = cumulative volume at bridging

QB = linear filtration rate at time of bridging

This is the case when both normal fluid loss and seepage occur. When total loss occurs, there is no
external filter cake formed and VB does not have a finite value. This equation is illustrated in Figure 35
for a suspension of silica flour on Berea sandstone.

As is seen from the figure, the slope is constant once the filter cake is formed. The values of tB, the
bridging time, and VB, the bridging volume, may be solved for by iteration from the general filtration
equation. In actuality, with PPT experiments at high pressure, the initial part of the curve is quite steep.
Due to the extremely short bridging time, normally on the order of a few seconds, sufficient quality data
is not available to accurately solve for tB and VB. The value reported, the spurt, is obtained by project-

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Figure 35
Example of Filton Curve with Invasion (from Barkman and Davidson)

ing the linear portion of the curve to the y-axis. In the example above the spurt is approximately
290 mL.

The slope of the linear portion of the curve, S, gives valuable information concerning the quality of the
filter cake. When S=0, an impermeable filter cake is formed. A large value of S indicates that a poor
quality filter cake is formed. The permeability of the cake is related to the slope by the following equa-
tion:

2ρ c k c A c2 ∆pt
S = -----------------------------------
-
µwρ w

where

ρc = bulk density of filter cake

kc = filter cake permeability

Ac = area of filter cake

pt = total pressure differential across filter cake and filter medium

µ = fluid viscosity

w = weight concentration of solids in water

ρw = density of fluid

As can readily be seen by examination of the equation, when only small changes are made to the fluid,
the slope varies as the square root of the filter cake permeability.

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Sized lost circulation materials (LCM) can also reduce cake thickness and filtration. Low permeability
filter cakes are the result of optimizing the distribution of sized solids in a mud. Low permeability filter
cakes not only reduce filtration, but also minimize differential pressure sticking. Commonly-used LCM’s
that reduce filtration are a variety of cullulosic material and sized solids calcium carbonate and gilso-
nite or similar material. Cellulosies are effective because of its ability to swell and physically bridge a
wide range of pore openings.

Pilot tests which use the PPT cell, rather than conventional HTHP filtration equipment can be used to
optimize additives and concentrations. Both PPT and conventional fluid loss tests should be performed
to identify trends and to evaluate the effectiveness of product treatments. (Figures 35 and 36 illustrate
how the PPT can be used to indicate improvements in the muds.) Running a PPT with every mud
check can direct mud treatments and thus minimize differential sticking tendencies.

Figure 36
Differential Pressure vs. PPT Fluid Loss
Field Mud Example - Gulf of Mexico
2 Darcy Disks Tested at 350°F

Table 16 contains PPT data which compare the effectiveness of various LCMs in a specific mud sys-
tem.

This table includes total leakoff, spurt, the slope of the linear portion of the volume versus the square
root of time curve and filter cake thickness for some runs. The last column consists of a value, the PPT
Value, that is reported by some sources. The value is defined as:

PPT Value = Spurt + 2 x [Total Volume (30 minutes) -Spurt]

The base mud is a water-based mud containing 20 ppb prehydrated bentonite, 30 ppb Rev-Dust,
0.5 ppb caustic, and 0.5 ppb PAC-L.

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Table 16
PPT Study of LCM Sealing on Aluoxite Disk

Total Slope,
PPT
Core Sample Leakoff, mL Spurt, mL mL/min Cake, 32nd
Value

AF-6 Base mud 23.56 1.91 3.95 45.2

AF-15 Base mud 25.71 1.71 4.38 - 49.71
AF-50 Base mud 55.45 33.55 4.00 77.34
FAO-50 Base mud 52.36 32.80 3.57 9 71.92
AF-50 Base mud - 35 ppb KCl 98.12 27.70 12.84 16 168.46
AF-50 Base mud - 10 ppb Baricarb 150 + 35.51 14.12 3.00 9 56.90
10 ppb Baricarb 6
FAO-50 Base mud 52.30 32.80 3.57 9 71.92
AF-50 Base mud + 10 ppb Ultra Seal XP 29.17 15.48 2.50 6 42.88
AF-50 Base mud + 10 ppb MIX 2 40.67 27.54 2.40 - 53.80
AF-80 Base mud Total Total No Cake No Cake -
AF-80 Base mud + 10 ppb Ultra Seal XP 72.85 30.80 2.19 - 94.85
AF-80 Base mud + 10 ppb MIX 2 Total Total No Cake No Cake -
AF-80 Base mud + 10 ppb Single Seal 100.75 34.50 2.77 - 124.91
AF-80 Base mud + 10 ppb Gran Seal 102.72 87.52 2.73 - 17.95
AF-80 Base mud + 15 ppb Kwik Seal Fine 69.47 51.47 3.29 - 87.47
+ 10 ppb Kwik Seal Medium + 5 ppb
Bore-Plate

If the core does not exhibit a high spurt, the material will not show its benefits as a seepage control
material but rather as a filter cake additive. As can be seen very little spurt was seen for AF-6 and
AF-15. Control here is provided by the filter cake which readily forms.
AF-50 did exhibit a significant spurt, but the solids in the base mud eventually bridged the pores and
allow a filter cake form. Addition of 35 ppb (10%) potassium chloride (KCl) did not change the spurt
appreciable but did increase the slope from 4.00 to 12.84. This is due to the flocculation of the bento-
nite in the mud which will deteriorate the filter cake. Addition of a sized calcium carbonate (BARA-
CARB) significantly decreased the spurt and caused negligible effect on the quality of the filter cake.
Two cellulosic materials are included for illustration. This series of tests does illustrate the changes
seen in the filter cake quality and fluid loss with different type additives.
The pores in AF-80 were large enough that no filter cake was formed during the base mud test. The
entire mud sample was passed through the core in a few seconds. This core was selected to run the
bulk of the tests for evaluation of the seepage control materials.
The best performance of the materials tested in the base mud was the ULTRA SEAL XP. This, at
10 ppb, gave results similar to the base mud containing 15 ppb KWIK-SEAL MEDIUM, 15 ppb
KWIK-SEAL FINE, and 5 ppb BORE-PLATE. GRAN SEAL and SINGLE SEAL gave similar, although
inferior, performance as evidenced by their higher spurt and total leakoff values when compared to the
ULTRA SEAL XP. MIX 2 failed to provide sufficient pore bridging to allow a filter cake to form.

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Permeability Plugging Test Procedure

The PPT apparatus may be used in the lab to evaluate lab formulated muds or mud systems submitted
by the field. The apparatus is also portable and can be used at the rig to evaluate the mud system and
to test the bridging effectiveness at downhole temperature and pressure of various additives. Informa-
tion from the PPT is especially useful on critical wells - drilling depleted sands or high angle holes. (A
diagram of the PPT apparatus is shown in Figure 37.) The test procedure is as follows:

[Note: Several manufacturers supply the hardware for the device. These steps are not meant to be
specific but rather apply to all cells. Manufacturer instructions should be consulted before any tests are
performed.]

Figure 37
Permeability Plugging Test Apparatus

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Step

1. Apply a thin coat of stopcock grease around the o-rings of the floating piston.

2. Screw the floating piston onto the T-bar wrench and install the piston into the bottom of the cell.
Work the piston up and down to ensure that it moves freely. (The bottom of the cell will have a
shorter recess than the top.) Position the piston so that it is near the bottom edge of the cell and
unscrew it from the wrench.

3. Install the hydraulic end cap onto the bottom of the cell.

4. Turn the cell upright and fill with 350 cm3 of mud.

5. Acceptable: Soak Aloxite disks for at least 5 minutes in fresh water prior to testing a water-based
mud. For oil muds, the Aloxite disks should be soaked in the representative base oil for at least
5 minutes prior to use.

Preferred: Place the aloxite disk in the appropriate solution. Place this in a vacuum cell and evacu-
ate for 1 hour.

Note: Aloxite disks should NEVER be reused.

6. Install the top cap with valve onto the cell. Close the valve and install the cell into the heating
jacket. Lower cell slowly until it bottoms out, then rotate clockwise until it locks in place.

7. Install a thermocouple in the small hole on the top of the cell.

8. Place the filtrate reservoir onto the top of the valve. Ensure that the small o-ring is in good condi-
tion. Lock reservoir in place by installing a safety key (modified cotter key).

9. Install the back pressure device onto the reservoir and lock in place with safety key.

10. Open the valve directly on top of the cell (green valve). Ensure that the other valves are closed on
the reservoir and backpressure devices.

11. Apply the appropriate amount of back pressure to the cell for the desired test temperature using
the CO2 backpressure device. (Refer to Table 17 for the recommended minimum backpressure.)
Once the backpressure is applied, close the valve on the cell (green valve) to trap the pressure.

12. Install the quick-connect from the hydraulic pump to the hydraulic end of the cell (bottom end).
Leave the black valve on the pump open.

13. Heat the cell to the desired temperature. Open the valve on the cell (green valve).

14. Close the valve on the pump (black valve) and apply desired pressure to the cell with the pump.

15. Once the desired pressure is applied, open the valve on the reservoir and collect the mud and/or
filtrate in a graduated cylinder. Continue to collect the liquid until the reservoir blows dry. This
should be recorded as the spurt loss.

16. Close the valve on the reservoir and maintain the desired pressure on the cell with the hydraulic
pump. (Most pumps leak slightly.) Hydraulic pressure will need to be applied to the cell to maintain
pressure on the cell for 30 minutes. Monitor the flow by bleeding the cell every 5 minutes and
recording the volume.

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Table 17
Recommended Minimum Back Pressure

Test Temperature Vapor Pressure Minimum Back Pressure

°F °C psi kPa psi kPa

212 100 14.7 101 100 690
250 121 30 207 100 690
300 149 67 462 100 690
LIMIT of Normal Field Testing
*350 177 135 932 160 1104
*400 204 247 1704 275 1898
*450 232 422 2912 450 3105
*DO NOT exceed equipment manufacturers’ recommendations for maximum tem-
peratures, pressures, and volumes.

17. After 30 minutes, record total amount of liquid recovered (exclude the spurt loss).

18. Release the pressure on the hydraulic pump and close the top valve.

19. Remove the hydraulic quick-connect from the cell to the pump.

20. Bleed off the back pressure. Remove back-pressure device and repeat the same for the reservoir.
Remove the reservoir from the top of the cell and clean.

21. Turn heating jacket off. Allow cell to cool by removing it from the heating jacket or cooling it in cold
water.

22. Open the top valve slowly to remove trapped pressure. Repeat this process several times to
ensure that all the pressure is removed from the cell.

23. Remove the top cap of the cell and turn the cell upside down. Remove the hydraulic end cap (bot-
tom cap) to expose the floating piston. Screw T-bar wrench into the piston and gently push down to
force mud and disk out the opposite end of the cell.

Note: This may cause mud to splatter out if too much pressure is applied.

24. Recover the Aloxite disk and filter cake. Wash cake very lightly with fresh water.

25. Measure filter cake thickness.

26. Preferred: Plot volume versus square root of time (minutes) and calculate spurt and S.

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Alternative: Total fluid loss is calculated as follows:

Note: Total Fluid Loss = (Spurt Loss, cm3) + [(2) (30 minute fluid recovery)]

The total fluid loss and filter cake thickness should be recorded daily on the mud sheet for trend
analysis. Whole mud and filtrate recovery should be differentiated in the spurt loss and 30 minute
recovery when possible.

27. Completely disassemble the cell and clean apparatus.

Pilot Testing
Introduction
Pilot testing of drilling fluids is testing performed on proportionately small-scale samples. It is an
essential part of drilling fluid testing and treating. Pilot testing minimizes the risk of sending a fluid
downhole that may be incompatible with the formations to be drilled or that may be ineffective under
downhole conditions. Generally, pilot testing is concentrated on the physical properties such as rheol-
ogy and fluid loss; however, it is important that chemical properties also be evaluated. Most chemical
reactions require heat, mixing, and time to drive the reaction. Therefore, it is necessary to have a
means for heating and agitating pilot test samples. Problems such as carbonates and bicarbonates are
not readily detectable and require a complete mud analysis and a pilot test series with heat aging to
determine proper treatment. Without heat aging, it is easy to overtreat the contaminant and create an
even more severe problem. A portable roller oven is a critical part of a pilot testing set-up at the rigsite.
A pilot test sample should be representative of the fluid being used. Pilot testing is thus based on the
fact that 1 g/350 cm3 of the sample is equivalent to 1 lb/bbl (42 gal) of the actual mud system. ( See
Figure 38 which illustrates pilot testing equivalents.)

Designing Pilot Tests

A pilot test or a series of pilot tests must be designed to answer the questions that you have in mind.
Therefore, it is necessary to know exactly the reason for the test. Some typical reasons are:

1. Mud response to downhole conditions, such as:

• temperature effects
• drilling uncured cement
• drilling anhydrite
• encountering salt/saltwater flows
• acid gas (CO2, H2S) intrusions
• water on water-based mud contamination in oil-based mud

2. Product response as a result of:

• purity, material variation (different lot #s)

• concentration
• compatibility with other components in the mud

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Figure 38
Pilot Testing Equivalents

• comparison to other products

• temperature/contamination
• shelf life

3. Adjustments to mud properties such as:

• weight up/dilution
• changing fluid loss properties
• changing alkalinity/pH
• treating carbonate/bicarbonate contamination
• reducing hardness
• adjusting MBT - clay content of the mud
• changing oil/water ratio of oil muds
• increasing electrical stability of oil muds

4. Study of effects of breakover, converting or displacement of muds, such as:

• displacing water-based mud with oil-based mud or vice versa

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• converting from freshwater mud to saturated salt mud

• breakover to lime or gyp mud
• reducing components in mud to convert to bland coring fluid
• treatment required to convert mud to a packer fluid
To determine how to design a pilot test or test series, look at economics and potential for problems
down the road. For example, if you expect to encounter a pressured saltwater flow (16 lb/gal) with a
15 lb/gal freshwater mud at 350°F, the parameters for testing could be: (1) maximum volume of saltwa-
ter anticipated in the mud, (2) weight up to 16 lb/gal with and without contaminant, (3) effects of tem-
perature on mud (15 and 16 lb/gal) with and without contamination, and (4) dilution and thinner
treatments.
Pilot test design requires calculating amounts of materials to put into the test samples. In pilot tests,
grams are equivalent to pounds and 350 cm3 is equivalent to one 42-gal oilfield barrel. Material bal-
ance equations, as developed in “Engineering”, are used for pilot test design. For example, to weight
the 15 lb/gal mud to 16 lb/gal without increasing the mud volume, one must calculate how much
15 lb/gal mud to dump and how much barite to add to increase density. For simpler pilot tests, such as
adding only a few lb/bbl treatment, it is not necessary to account for material balance.

Note: For liquid additives, volumes (gallons, buckets, drums) must be converted into weights
(pounds, grams) for pilot testing.

Rigsite pilot tests have distinct practical advantages over sending a mud into the laboratory or having a
laboratory mud prepared for pilot testing. Rigsite testing allows actual material and mud to be used,
which allows results to be readily available. quicker (which is usually very important), and allows rig
supervisor and mud engineer to evaluate and review the pilot test results.
Laboratory pilot tests and planning are both important in preparing to drill a troublesome well. Both
should be done long in advance of anticipated problems. In this case, lab pilot tests are advantageous
in that they can be performed in advance, but then pilot tested again at the rigsite with the actual mud
and chemicals.

Note: Protective eyewear (safety glasses or safety goggles) must be worn at all times when mix-
ing chemicals.

Pilot Testing Equipment

A balance that can weight from 0.1 to 300 g and an oven (preferably roller oven) that can go to approx-
imately 400°F are needed. Mud cells (three minimum) made of stainless steel to hold at least 300 cm3
of mud at 1000 psi, a mixer such as a Hamilton Beach mixer are also needed. Mud testing equipment
that is accurately calibrated, along with fresh reagents for titrations are essential for pilot testing. Most
mud companies can provide a Pilot Test Kit; they do not usually contain the oven and cells, but are
available upon request.

Interpretation of Pilot Test Results

A single pilot test can give only limited information, but this is often sufficient for the need. Most often a
series of pilot tests (three to five samples) are required to properly answer the questions. For every

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Table 18
Specific Gravity of Common Drilling Fluid Components

Material Specific Gravity lb/gal lb/bbl

Fresh Water 1.00 8.33 350
Seawater 1.03 8.58 361
Diesel Oil #2 0.84 7.0 294
Saturated Saltwater 1.20 10.0 420
API Bentonites 2.60 21.6 910
Calcium Carbonate, CaCO3 2.75 22.9 963
Caustic Soda*, NaOH 2.13 17.7 525
Lime, Ca(OH)2 2.20 18.3 746
Lignite 1.50 12.5 525
Gypsum CaSO4.2H 2O 2.30 19.2 805
Lignosulfonate 0.83 6.9 290
Soda Ash, Na2CO3 2.53 21.1 886
Salt, NaCl 2.16 18.0 756
lb
Volume Increase = ---------------- = bbl increase
lb/bbl

*Caustic Soda 50% Solution

1 cm3/350 cm 3 = 1/2 lb/bbl
2 cm3/350 cm 3 = 1 lb/bbl

pilot test (single or series) a control sample must be run along in parallel with the test sample. A control
sample is the base mud which has not been treated, but which is taken through all the mixing, heating,
rolling, etc. processes. The control is used to aid interpretation of results. Data are compared between
the control and test sample to sort out the effects due to treatment versus mechanical effects (mixing,
rolling or time of exposure). For example, a mud engineer has an oil mud with a low electrical stability
(ES). He pilot tests a sample with 2 lb/bbl (2 g/350 cm3) additional emulsifier and shears it on the mixer
for 10 minutes. The ES is much higher than before. He also has run a control sample on the mixer for
10 minutes, but without the additional emulsifier, and obtained almost the same higher ES. Was the
emulsifier responsible for the improved ES? No, in this case the shearing was what gave the improve-
ment.
Results of pilot testing should be thoroughly reviewed before drawing conclusions. Often, a pilot will
lead to another one or two tests before the answer is satisfactorily clear.

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Figure 39
Weighing Equipment

Figure 40
Mixing Equipment

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