W.B.M & O.B.M Testing PDF

CHAPTER
3 Testing
Water-Mud Testing ............................................................................................. 3.3

Section 1. Density of Fluid (Mud Weight) .............................................................. 3.3
Section 2. Viscosity ............................................................................................................ 3.4
A) Marsh Funnel .......................................................................................................................... 3.4
B) Rotational Viscometer ............................................................................................................ 3.5
Section 3. Filtration ........................................................................................................... 3.7
A) API Fluid Loss ......................................................................................................................... 3.7
B) High-Temperature, High-Pressure (HTHP) Filtration ............................................................ 3.8
C) Filter-Cake Compressibility .................................................................................................. 3.11
Section 4. Sand Content ................................................................................................ 3.11
Section 5. Liquid and Solid Content ....................................................................... 3.12
A) Procedure: Retort ................................................................................................................. 3.12
B) Methylene Blue Capacity ..................................................................................................... 3.14
C) Methylene Blue Capacity of Shale ...................................................................................... 3.14
D) Flocculent Efficiency Test .................................................................................................... 3.15
Section 6. Hydrogen Ion Concentration (pH) .................................................... 3.15
A) Indicator Sticks ..................................................................................................................... 3.15
B) pH Meter ............................................................................................................................... 3.16
Section 7. Chemical Analysis of Water-Base Drilling Fluids ........................ 3.17
A) Alkalinity (Pf, Mf, Pm and Lime Content) ........................................................................... 3.17
B) Garrett Gas Train (GGT) Test for Carbonates ...................................................................... 3.19
C) Chloride (Cl–) ........................................................................................................................ 3.21
D) Calcium — Qualitative ........................................................................................................ 3.22
E) Total Hardness ....................................................................................................................... 3.22
F) Hardness in Dark Filtrates ..................................................................................................... 3.23
G) Sulfate ................................................................................................................................... 3.25
H) Potassium (K+) ....................................................................................................................... 3.26
I) Nitrate Ion Concentration .................................................................................................... 3.28
J) PHPA Polymer Concentration ............................................................................................... 3.30
Section 8. Chemical Analysis Relating to Corrosion ...................................... 3.32
A) Zinc oxide (ZnO) and Basic Zinc Carbonate (ZnCO3•Zn(OH)2) ....................................... 3.32
B) Iron Sulfide Scale (Qualitative) ............................................................................................ 3.33
C) Hydrogen Sulfide (H2S) ....................................................................................................... 3.33
D) Phosphate ............................................................................................................................. 3.35
E) Oxygen Scavenger: SO32– Content ........................................................................................ 3.38
Section 9. Resistivity ....................................................................................................... 3.39
Section 10. Glycol Testing Procedure ..................................................................... 3.40
A) Refractometer ........................................................................................................................ 3.40
B) Dual-Temperature Retort Analysis for Glycol Systems ....................................................... 3.40
C) Chemical Determination of Glycol Using Centrifuge ....................................................... 3.41
Section 11. KLA-GARDT Concentration ..................................................................... 3.41
Testing 3.1 Revision No: A-1 / Revision Date: 02·28·01

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3 Testing
Section 12. Permeability Plugging Test Procedure ........................................... 3.43

Section 13. Brookfield Viscometer ........................................................................... 3.45
Section 14. Drill Pipe Corrosion Ring Coupons ................................................ 3.48
A) Ring Coupon Monitoring Procedure ................................................................................... 3.49
B) Laboratory Coupon Analysis ................................................................................................ 3.49
C) Calculation of Corrosion Rates ............................................................................................ 3.50
Oil-Mud Testing (Including Diesel Oil,

Mineral Oil and Synthetic Fluids) .............................................. 3.52
Section 1. Aniline Point Determination ............................................................... 3.52
Section 2. Density (Mud Weight) .............................................................................. 3.52
Section 3. Viscosity and Gel Strength .................................................................... 3.53
A) Marsh Funnel ........................................................................................................................ 3.53
B) Rotational Viscometer .......................................................................................................... 3.53
Section 4. Filtration ......................................................................................................... 3.55
Section 5. Activity ............................................................................................................ 3.57
Section 6. Electrical Stability ...................................................................................... 3.57
Section 7. Liquid and Solids ........................................................................................ 3.58
Section 8. Chemical Analysis of Oil-Base Drilling Muds .............................. 3.59
A) Alkalinity (Pom) (VSA•API) ................................................................................................... 3.59
B) Salinity — Chlorides in the Whole Mud ............................................................................. 3.59
C) Whole Mud Calcium Calculation ....................................................................................... 3.60
D) Sulfides .................................................................................................................................. 3.60
Pilot Testing ............................................................................................................... 3.63

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3 Testing
Water-Mud Testing
The API has recommended standard Water-Based (Oil-Based) Drilling Fluids,”
methods of conducting field and labora- API RP 13B-1, 13B-2 and supplements
tory tests for drilling fluids and detailed (also see 13I for Laboratory Testing
procedures may be found in the API Drilling Fluids, 13J for Testing Heavy
publication, “Recommended Practice: Brines and supplements).
Standard Procedure for Field Testing
Section 1. Density of Fluid (Mud Weight)
Instruments
The density (commonly referred to as
mud weight) is measured with a mud
balance of sufficient accuracy to mea-
sure within 0.1 lb/gal (0.5 lb/ft3 or 5 psi/
1,000 ft of depth). For all practical pur-
poses, density means weight per unit
volume and is measured by weighing
the mud. The weight of mud may be
Figure 1: M-I mud balance.
expressed as a hydrostatic pressure gra-
dient in lb/in.2 per 1,000 ft of vertical Calibration
depth (psi/1,000 ft), as a density in 1. Remove the lid from the cup and
lb/gal, lb/ft3 or Specific Gravity (SG) completely fill the cup with pure
(see Table 1). or distilled water.
2. Replace the lid and wipe dry.
lb/gal lb/ft3 g 3. Replace the balance arm on the
SG = or or base, with the knife edge resting
8.345 62.3 cm3
on the fulcrum.
4. The level-bubble should be centered
Table 1: Conversion table for density units.
when the rider is set on 8.33 lb/gal.
MUD BALANCE If not, adjust using the calibration
Description screw in the end of the balance arm.
Some balances do not have calibra-
The mud balance (see Figure 1) con-
tion screws and must have lead
sists principally of a base on which
shot added or taken out through
rests a graduated arm with cup, lid,
the calibration cap.
knife edge, level vial, rider and coun-
terweight. The constant volume cup is Procedure
affixed to one end of the graduated 1. Remove the lid from the cup, and
arm, which has a counterweight at the completely fill the cup with the
other end. The cup and arm oscillate mud to be tested.
in a plane perpendicular to the hori- 2. Replace the lid and rotate until
zontal knife edge, which rests on the firmly seated, making sure some
support, and are balanced by moving mud is expelled through the hole
the rider along the arm. in the lid.
3. Wash the mud from the outside of
the cup, and dry it.

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3 Testing
4. Place the balance arm on the base, Mud gradient:

with the knife edge resting on the psi/ft = 0.052 x lb/gal
fulcrum. = 0.4333 x SG
5. Move the rider until the graduated = 0.00695 x lb/ft3
arm is level, as indicated by the SG
level vial on the beam. kg/cm2/m =
10
6. At the edge of the rider closest to 141.5
the cup, read the density or weight SG at 60°F (15.6°C) =
131.5 + °API
of the mud.
7. Report the result to the nearest scale Where:
division, either in lb/gal, lb/ft3, °API = American Petroleum
psi/1,000 ft of depth or Specific Institute gravity
Gravity (SG).
8. For balances not showing the
desired scale, the equations shown
in Table 1 may be used.
Section 2. Viscosity
Instruments
The Marsh funnel is used for routine
field measurement of the viscosity of
drilling mud. The Fann V-G meter is
used to supplement the information
obtained from the Marsh funnel, par-
ticularly with respect to the gel char-
acteristics of the mud. The V-G meter
is capable of giving the apparent vis-
Figure 2: Marsh funnel.
cosity, plastic viscosity, yield point
and gel strengths (initial and timed). Calibration
A) MARSH FUNNEL Fill the funnel to the bottom of the
Description screen (1,500 ml) with freshwater at
70±5°F. Time of outflow of 1 qt (946 ml)
The Marsh funnel (see Figure 2) is
should be 26 sec ±0.5 sec.
6 in. in diameter at the top and 12 in.
long. At the bottom, a smooth-bore Procedure
tube 2 in. long having an inside diam- 1. With the funnel in an upright posi-
eter of 3⁄16 in. is attached in such a way tion, cover the orifice with a finger
that there is no constriction at the joint. and pour the freshly collected mud
A wire screen having 1⁄16-in. openings, sample through the screen into a
covering one-half of the funnel, is clean funnel until the fluid level
fixed at a level of 3⁄4 in. below the reaches the bottom of the screen
top of the funnel. (1,500 ml).

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3 Testing
2. Immediately remove the finger Torsion spring constant

from the outlet and measure the 386 dyne-cm/degree deflection
time required for the mud to fill Rotor speeds: High speed: 600 RPM
the receiving cup to the 1-qt mark Low speed: 300 RPM
on the cup.
The following are types of viscome-
3. Report the result to the nearest
ters used to test drilling fluids:
second as Marsh funnel viscosity.
1. Hand-cranked instrument has speeds
Report fluid temperature in degrees
of 600 and 300 RPM. A knob on the
Fahrenheit or Centigrade.
hub of the speed-change lever is
B) ROTATIONAL VISCOMETER used to determine gel strength.
Description 2. The 12-volt, motor driven instru-
Direct-indicating viscometers are rota- ment also has speeds of 600 and
tional types of instruments powered 300 RPM. A governor-release switch
by an electric motor or a hand crank. permits high shearing before meas-
Drilling fluid is contained in the annu- urement, and a knurled hand-wheel
lar space between two concentric cylin- is used to determine gel strength.
ders. The outer cylinder or rotor sleeve 3. The 115-volt instrument (see Figure 3)
is driven at a constant RPM (rotational is powered by a two-speed synchro-
velocity). The rotation of the rotor nous motor to obtain speeds of 600,
sleeve in the fluid produces a torque 300, 200, 100, 6 and 3 RPM. The
on the bob or inner cylinder. A torsion 3-RPM speed is used to determine
spring restrains the movement of the gel strength.
bob, and a dial attached to the bob
indicates displacement of the bob.
Instrument constants have been
adjusted so that plastic viscosity and
yield point are obtained by using
readings from rotor sleeve speeds
of 600 and 300 RPM.
Specifications: Direct-indicating
viscometer
Rotor sleeve
Inside diameter 1.450 in. (36.83 mm)
Total length 3.425 in. (87.00 mm)
Scribed line 2.30 in. (58.4 mm)
above the bottom
of sleeve.
1
Two rows of ⁄8-in. (3.18-mm) holes
spaced 120 degrees (2.09 radians) apart,
around rotor sleeve just below scribed Figure 3: V-G meter laboratory model.
line. 4. The variable speed 115- or 240-volt
Bob instrument is powered to obtain all
Diameter 1.358 in. (34.49 mm) speeds between 625 and 1 RPM. The
Cylinder length 1.496 in. (38.00 mm) 3-RPM speed is used to determine
Bob is closed with a flat base and a gel strength.
tapered top.

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3 Testing
1) PROCEDURE FOR APPARENT VISCOSITY, 2) PROCEDURE FOR GEL

PLASTIC VISCOSITY AND YIELD POINT STRENGTH DETERMINATION
DETERMINATION 1. Stir sample at 600 RPM for approxi-
1. Place recently agitated sample in mately 15 sec and slowly lift the gear
a thermocup and adjust surface assembly to the neutral position.
of mud to scribed line on the 2. Shut motor off and wait 10 sec.
rotor sleeve. 3. Flip switch to the low-speed position
2. Heat or cool the sample to 120°F and record maximum deflection
(49°C). Stir slowly while adjusting units in lb/100 ft2 as initial gel. If the
the temperature. dial indicator does not return to zero
3. Start the motor by placing the with motor off, do not reposition.
switch in the high-speed position 4. Repeat 1 and 2, but allow 10 min,
with the gear shift all the way then place switch in the low-speed
down. Wait for a steady indicator position and read maximum deflec-
dial value, and record the 600 RPM tion units as the 10-min gel. Report
reading. Change gears only when measured temperature.
motor is running. Care of Instrument
4. Change switch to the 300-RPM Clean instrument by running at high
speed. Wait for a steady value and speed with rotor sleeve immersed in
record 300-RPM reading. water or other solvent. Remove rotor
5. Plastic viscosity in centipoise = sleeve by twisting slightly to release
600 reading minus 300 reading lock pin. Wipe bob and other parts
(see Figure 4). thoroughly with clean, dry cloth or
6. Yield Point in lb/100 ft2 = 300 reading paper towel.
minus plastic viscosity in centipoise. CAUTION: The bob is hollow and can
7. Apparent viscosity in centipoise = be removed for cleaning. Moisture will
600 reading divided by 2. occasionally collect within the bob and
should be dried out with a pipe cleaner.
u600 Immersion of the hollow bob in extremely
Slope = plastic hot mud (>200°F) could result in a very
viscosity dangerous explosion.
Deflection (dial units)
u300 NOTE: Never immerse meter in water.
Intercept =
yield point
300 600
Speed (rpm)
Figure 4: Typical flow curve for a drilling mud.

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3 Testing
Section 3. Filtration
Description
The filtration or wall-building prop-
erty of a mud is determined by means
of a filter press. The test consists of
determining the rate at which fluid is
forced through the filter paper. The
test is run under specified conditions
of time, temperature and pressure.
The thickness of the solid filter cake
deposited is measured after the test.
The filter press being used should
meet specifications as designated in the
API Recommended Practice and con-
ducted in the manner suggested. The
API fluid loss is conducted at surface
temperature at 100 psi pressure, and is
recorded as the number of milliliters
lost in 30 min.
Instruments
Figure 5: An example of an API filter press.
This instrument (see Figure 5) consists
of a mud cell assembly, pressure regu- A) API FLUID LOSS
lator and gauge mounted on the top of Procedure
the carrying case or the top part of the 1. Have air or gas pressure of 100 psi
car laboratory unit. The cell is attached available.
to the regulator by means of a coupling 2. Remove the lid from the bottom
adapter by simply inserting the male of the clean and dry cell. Place the
cell coupling into the female filter press O-ring in an undamaged groove,
coupling and turning clockwise 1⁄4 turn. then invert to fill. Any mechanical
Some cells do not have this locking damage could prevent it from sealing.
device, and are just inserted into the Seal the inlet with a finger.
proper coupling. The cell is closed at 3. Fill the cell with mud to within
the bottom with a lid fitted with a 1
⁄4 inch of O-ring groove. Place filter
screen (or grid), by placing the lid paper (Whatman No. 50 or equiva-
firmly against the filter paper and lent) on top of O-ring. Place the lid
turning to the right until hand tight. on the filter paper with the flanges
This forces the sheet of filter paper of the lid between the flanges of the
against the O-ring previously fitted in cell, and turn clockwise until hand
the base of the cell. Pressure is sup- tight. Turn the cell over and insert
plied by a small cartridge of carbon the male cell coupling into the
dioxide gas. A bleed-off valve is pro- female filter press coupling and
vided to release the pressure prior to turn either direction to engage.
uncoupling the cell. Do not use N2O, 4. Place a suitable graduated cylinder
nitrous oxide (Whippets). under the filtrate opening to receive
the filtrate.

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3 Testing
5. Open the inlet valve applying pres-

sure to the cell. (A rapid fluctuation
downward of the needle can be
seen as pressure fills the cell.)
6. The normal API test period is
30 min. At the end of the test,
close the valve. Pressure will be
shut off at the source, and the
pressure will bleed off auto-
matically. Remove the cell.
7. Report the fluid loss in milliliters
unless otherwise specified.
8. Disassemble the cell, discard the mud
and use extreme care to save filter Figure 6: HTHP filter press (disassembled).
paper with a minimum of distur-
bance of the cake. Wash the cake gen- 13. Take the mud from the flow line and
tly to remove excess mud. Measure fill to within 1⁄2 in. of the O-ring
the thickness of the filter cake and groove to allow for expansion.
report in 32nds of an inch. 14. Place one circle of filter paper in
groove and place the O-ring on
B) HIGH-TEMPERATURE,
top of paper. Use Whatman No. 50
HIGH-PRESSURE (HTHP) FILTRATION
paper or equivalent.
MB style (API #II) HTHP filter press 15. Place the cell plate assembly over
Description the filter paper and align the safety
The instrument (see Figures 6 and 7) locking lugs.
consists of a heating jacket with ther- 16. Evenly tighten cap screws finger
mostat, cell plate assembly, primary tight and close the discharge valve.
pressure assembly and back-pressure 17. With cell plate assembly down, place
receiver. The capacity of the mud cell cell in heating jacket with all valves
is 160 ml with a filter area of 3.5 in.2. closed. Transfer the thermometer to
Filtrate receiver holds 15 ml, and up the cell’s thermometer well.
to 100 psi backpressure can use a glass 18. Place CO2 cartridge in primary pres-
tube. If a higher back pressure is to be sure assembly and tighten cartridge
used, a stainless-steel tube should holder until cartridge is punctured.
replace the glass. The regulator and bleed-off valve
A routine test can be conducted at should be closed.
300°F and 500 psi differential pressure. 19. While lock ring is lifted, slide pri-
High-temperature fluid loss is recorded mary pressure assembly onto the
as double the number of milliliters lost top “slide coupling” and release
in 30 min. the lock ring.
Procedure 10. Place 100 psi pressure on top
11. Plug heating jacket cord into proper valve, then open it to pressurize
power source and allow instru- unit. This pressure will minimize
ment to preheat. Place thermom- boiling while sample is heating.
eter in well in heating jacket and 11. Always use the back-pressure
adjust thermostat to obtain 10°F receiver to prevent vaporization
above desired test temperature. of the filtrate at test temperatures
12. Close the inlet valve on the cell near boiling or higher. Place and
and invert the cell. activate a CO2 cartridge into the
back-pressure receiver assembly.

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3 Testing
12. Slide back-pressure assembly into 21. Invert cell, loosen cap screws (use
place with slotted lock ring. Allen-head wrench if necessary)
13. Apply 100 psi pressure to the bot- and disassemble. Thoroughly
tom pressure unit with this valve clean and dry all parts.
still closed.
API #I STYLE HTHP FILTER PRESS
14. After the temperature has reached
(HOLLOW TAPERED-TIP STEM)
the desired range (300°F), as noted
by the cell thermometer, increase The standard HTHP fluid loss test is
pressure on top cell regulator from run at a temperature of 300°F (148°C)
100 to 600 psi while maintaining and a differential pressure of 500 psi.
100 psi on the bottom regulator. Description
Open bottom cell valve one turn, 1. Heating jacket mounted on a stand.
and start timing test. 2. A sample cell rated to a working
15. Maintain 100 psi on the receiver pressure of 1,000 psi (filter area of
during the test. If it rises, drain 3.5 in.2).
a little filtrate to maintain the 3. Thermometer or electronic thermo-
500 psi differential. Maintain couple (readings to 500°F [260°C]).
temperature ±5°F. 4. Top assembly regulator with the
16. After 30 min filtration, close bot- ability to regulate 1,000 psi from
tom cell valve and then close top any pressure source used.
cell valve. 5. Filtrate receiver (100 ml recom-
17. Back off both regulator T-screws and mended) designed to withstand a
bleed pressure from both regulators. working back pressure of at least
18. Drain filtrate into graduated cylin- 500 psi.
der and read volume. Double the 6. Graduated cylinder for filtrate
reading to report. Remove receiver. collection.
19. Disconnect primary pressure NOTE: Extreme caution should be used
assembly by lifting lock ring and in running an HTHP test. Maintain all
slip assembly off. equipment in a safe working condition.
CAUTION: Cell still contains pressure. Testing at temperatures of 300°F
20. Maintain cell in upright position (149°C) or less
and cool to room temperature, then 11. Plug heating jacket into correct
bleed off cell pressure; do not blow voltage for the unit. Place ther-
mud through valve. mometer in the thermometer well
on the outside of jacket.
12. Preheat jacket to 10°F above the
test temperature and maintain if
needed, by adjusting the thermo-
stat. Check all O-rings and replace
as needed.
13. Agitate the mud sample for 10 min
and pour into the cell making sure
the valve stem on the cell body is
closed. The cell should not be filled
closer than 1⁄2 in. from the top of
the lip.
14. Place a piece of filter paper
(Whatman No. 50 or equivalent)
on top of the lip.
Figure 7: HTHP filter press (MB style - API #II).

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3 Testing
15. Seat lid properly, align and tighten

Allen screws. Make sure that both
valve stems are closed and then
place the cell into the heating
jacket. With a twisting motion
lock the cell in the jacket.
NOTE: The cell body fits in the
jacket with the end containing the
filter paper on the bottom.
16. Transfer the thermometer to the
cell body thermometer well.
17. Place the pressure unit on the top
valve and lock into place with a
locking pin.
18. Place the bottom low-pressure
receiver to the bottom valve and
lock into place (see Figure 8).
19. Apply 100 psi to both pressure
units and open top valve stem
1
⁄4 turn counterclockwise.
10. When the test temperature is
reached, increase the pressure of the Figure 8: HTHP filter press (API #I style) (disassembled).
top pressure unit to 600 psi and open Remove the cell from the heating
the bottom valve stem 1⁄4 turn clock- jacket and cool to room temperature
wise to begin filtration. The filtrate in an upright position.
is to be collected in a graduated CAUTION: Cell still contains pressure.
cylinder for a period of 30 min. 13. While allowing the cell to cool,
11. While testing, the test temperature measure the amount of collected
should be maintained within ±5°F. filtrate and double the results.
Drain some filtrate when the back Record as milliliters of filtrate
pressure exceeds 100 psi. along with the test temperature.
12. After 30 min close both valves and 14. After the cell has cooled, bleed the
back the regulator T-screws off. Bleed pressure carefully from the top stem
the filtrate and pressure from the opposite the filter paper. Close the
bottom receiver and then bleed the valve and then open the other end
pressure from the top regulator. carefully to bleed off any pressure.
Remove top regulator and receiver.
Coefficient of
Volume Expansion
for Water at
Saturation Suggested Applied
Aging Temperature Water Vapor Pressure Pressure Back Pressure
°F °C kPa psi kPa psi
212 100 101 14.7 1.04 689 100
250 121 207 30 1.06 689 100
300 149 462 67 1.09 689 100
350 177 931 135 1.12 1,104 160
400 205 1,703 247 1.16 1,898 275
450 232 2,917 422 1.21 3,105 450
Note: Do not exceed equipment manufacturer’s recommendations for maximum temperatures, pressures and volumes.
Table 2: Vapor pressure and volume expansion of water between 212 and 450°F with suggested back pressure.

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3 Testing
Disassemble after there is no remain- 2. Temperatures over 350 to 400°F

ing pressure, and discard mud sam- require the use of porous stainless-
ple. Visually observe and note the steel disc (Dynalloy X5 or equiva-
condition of the filter cake. It can lent) in place of filter paper (see
be measured in 1⁄32 of an inch. API RP 13B-1 and 13B-2).
Testing at temperatures between 3. Time for heating sample should
300 to 400°F (149 to 233°C) not exceed 1 hour.
The same basic procedure is used except C) FILTER-CAKE COMPRESSIBILITY
the 500-ml cell and nitrogen pressure The test is run using the same proce-
manifold is suggested: dure at 300°F (149°C), but 200 psi is
1. When heating the sample, 450 psi applied to the cell body and 100 psi
can be placed on both pressure is applied to the bottom receiver. The
units. When the test begins, the top 100 and 500 psi differential values
pressure is raised to 950 psi and the are compared.
bottom pressure is maintained at
450 psi.
Section 4. Sand Content

Instruments to be added in order to read the per-
The sand content of mud is estimated centage of sand directly in the bottom
by the use of a sand-screen set. The of the tube, which is graduated from
screen test, because of its simplicity of 0 to 20%.
operation, is widely used in the field. Procedure
1. Fill the glass measuring tube to the
indicated mark with mud. Add water
to the next mark. Cover the mouth
of the tube with the thumb and
shake vigorously.
2. Pour the mixture onto the screen,
add more water to the tube, shake
and again pour onto the screen.
Repeat until the wash water is clear.
Figure 9: Sand content set. Wash the sand clean that is retained
on the screen.
SAND CONTENT SET 3. Fit the funnel down over the top of
Description the sieve. Insert the tip of the funnel
The sand content set (see Figure 9) into the mouth of the glass tube.
consists of a 21⁄2-in. diameter sieve, Wash the sand from the screen into
200 mesh (74 micron), a funnel to the tube by means of a fine spray of
fit the sieve and a glass measuring water. Allow the sand to settle. From
tube marked for the volume of mud the graduations on the tube, read the
percent by volume of sand.

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3 Testing
Section 5. Liquid and Solid Content

Instruments
A mud retort with “oven” heating
capability is used to determine the
quantity of liquids and solids in a drill-
ing fluid. Internal-probe heater retorts
are not recommended. A sample of
mud (either 10-, 20- or 50-ml retorts
are available) is placed in the cup and
the lid added to expel some fluid. This
ensures a correct volume. It is heated
until the liquid components have
been vaporized. The vapors are passed
through a condenser and collected in
a graduated cylinder that usually is grad-
uated in percent. The volume of liquid,
oil and water, is measured directly in Figure 10: Retort.
percent. The solids, both suspended
and dissolved, are determined by sub- 5. Plug power cord into the correct
tracting from 100% or by reading the voltage and keep power on until
void space at the top. distillation stops, which may
require 25 min depending on the
Description characteristics of oil, water and
A) PROCEDURE: RETORT solids content.
1. Allow the mud sample to cool to 6. Allow the distillate to cool to
room temperature. room temperature.
2. Disassemble retort assembly and 7. Read the percentage of water, oil and
lubricate sample cup threads with solids directly from the graduate. A
high-temperature grease (Never- drop or two of aerosol solution will
SeezT). Fill sample cup almost level help define the oil-water interface,
full of the fluid to be tested. Put sam- after reading the percent solids.
ple cup cover in place by rotating 8. At end of the test, cool completely,
firmly, squeezing out excess fluid then clean and dry retort assembly.
to obtain the exact volume — 10, 9. Run a pipe cleaner through condenser
20 or 50 ml required. Clean spills hole and retort drain tube to clean
from cover and threads. and maintain full openings. NOTE:
3. Pack fine steel wool into the upper Do not allow drain tube to become
expansion chamber, then screw restricted.
sample cup into expansion cham-
Percent by volume solids analysis,
ber. The steel wool should trap the
weight method (calculation by weight
solids boiled out. Keep assembly
difference using conventional retort)
upright so that mud does not flow
1. Equipment needed:
into the drain tube.
Mud balance.
4. Insert or screw the drain tube into
Conventional 20 cm3
hole at end of condenser, seating
(oven-type) retort.
firmly. The graduated cylinder
Analytical balance accurate
which is calibrated to read in per-
to 0.01 g.
cent should be clipped in place on
the condenser.

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3 Testing
2. Four measurements are taken: 2. Disassemble retort and add mud to

A. Mud weight. fill sample cup. Measurement of
B. Weight of retort (including steel volume or use of lid is unnecessary
wool and cup). as volumes are calculated in this
C. Weight of retort with whole mud. weigh-in/out procedure. Weigh the
D. Weight of retort with mud solids. reassembled retort. This is value C.
Procedure 3. Run retort as usual collecting
1. Ready the retort with steel wool distillate (water and any oil).
and sample cup. Determine the 4. Allow the retort to cool and
weight in grams. This is value B. reweigh the assembly. This is
value D.
Calculation
Calculate:
1. Mud density (g/cm3); SGMUD = mud wt (lb/gal) x 0.11994.
2. Grams of mud in retort: g of mud = Value C – Value B.
3. Grams or cm3 water distilled: Value C – Value D.
Compute volume % solids:
(C – B) – SGMUD x (C – D)
Fraction of solids =
C–B
% solids = 100 x volume fraction solids
Example:
Four measurements from a field mud:
A) 12.70 lb/gal
B) 317.45 g
C) 348.31 g
D) 332.69 g
Thus:
#1 = 12.70 lb/gal [0.1194 g/cm3
lb/gal ] = 1.523 g/cm 3
#2 = 348.31 – 317.45 = 30.86 g of mud

#3 = 348.31 – 332.69 = 15.62 g of water
30.86 – 1.52 x 15.62
Volume fraction solids =
30.86
7.12
Fraction of soli =
30.86
Fraction of solid = 0.2307
% solids = 100 x 0.2307 = 23.07%

CHAPTER
3 Testing
B) METHYLENE BLUE CAPACITY the flask with a glass rod and place
Field procedure for determining on filter paper. The endpoint of the
cation exchange capacity titration is reached when the dye
Equipment appears as a greenish-blue ring sur-
1. Syringe, 3 ml, burette 10 ml. rounding the dyed solids.
2. Micropipette, 0.5-ml. 3. When the greenish-blue tint spread-
3. Erlenmeyer flask, 250-ml ing from the spot is detected, shake
with rubber stopper. the flask an additional 2 min and
4. Burette or pipette, 10-ml. place another drop on the filter
5. Graduated cylinder, 50-ml. paper. If the greenish-blue ring is
6. Stirring rod. again evident, the endpoint has
7. Hot plate. been reached. If the ring does not
8. Filter paper: 11 cm diameter, appear, continue as before until a
Whatman No. 1 or equivalent. drop taken after shaking 2 min
shows the greenish-blue tint.
Reagents
4. Record the ml of methylene blue
1. Methylene blue solution:
solution used.
1 ml = 0.01 milliequivalents
5. Methylene blue capacity of mud
3.74 g USP-grade methylene blue
English system MBC (lb/bbl) =
(C16H18N3SCl•3H2O) per liter.
(cm3 of methylene blue/cm3 of
2. Hydrogen peroxide, 3% solution.
mud) x 5
3. 5 N sulfuric acid solution.
Metric system MBC (kg/m3) =
Procedure (cm3 of methylene blue/cm3 of
1. Add 2 ml of mud (or suitable vol- mud) x 14
ume of mud to require 2 to 10 ml
of reagent) to 10 ml of water in the C) METHYLENE BLUE CAPACITY
Erlenmeyer flask. Add 15 ml of 3% OF SHALE
hydrogen peroxide and 0.5 ml of Methylene blue capacity
5 N sulfuric acid solution and mix (bentonite equiv.)
by swirling before heating. Boil English system MBC (lb/bbl) = CEC x 5
gently for 10 min. Dilute to about Metric system MBC (kg/m3) = CEC x 14
50 ml with water. NOTE: Drilling Cation exchange capacity
muds frequently contain substances in for shales
addition to bentonite that absorb meth- Approximately 1 g of dried ground
ylene blue. Treatment with hydrogen shale is accurately weighed and placed
peroxide is intended to remove the in a 150-ml Erlenmeyer flask and 50 ml
effect of organic materials such as of deionized water is added. The shale
CMC, polyacrylates, lignosulfonates slurry is gently boiled with 0.5 ml 5 N
and lignites. sulfuric acid for 10 min. The slurry is
2. Add methylene blue solution, allowed to cool and is titrated in 0.5 ml
0.5 ml at a time, from the burette increments with 0.01 N methylene
or pipette to the flask. After each blue solution.
addition, insert rubber stopper and
shake contents of the flask for CEC in milliequivalents/100 g shale =
about 30 sec. While the solids are ml of methylene blue
still suspended, remove a drop from g of shale titrated

CHAPTER
3 Testing
D) FLOCCULENT EFFICIENCY TEST flocculent would not be required at

Procedure that time. Repeat this test daily or
1. Measure 100 ml of drill water every other day.
directly from rig flow line into a 6. The flocculent with the fastest time
graduated cylinder. is the correct one to use.
2. Add 1 ml of 1%* flocculent solution NOTE: To determine if flocculent is
to the graduated cylinder. needed in clear water drilling, collect
3. Invert the graduated cylinder slowly 3 a sample of water where it returns to the
to 4 times and set it on a flat surface. suction pit and run a floc test.
4. Record the time (in sec) required *1% flocculent solutions are made by
to form the flocs and settle to the adding 1 g of the correct flocculent
40 cm3 line on the graduated cylinder. to 100 ml of distilled water and stirring
5. Repeat the procedure with each until dissolved.
flocculent. If no flocs form, then a
Section 6. Hydrogen Ion Concentration (pH)

Purpose dependent on the pH of the fluid in
Field measurement of drilling fluid which the stick is placed. Standard
(or filtrate) pH and adjustments to the color charts are supplied for compari-
pH are fundamental to drilling fluid son with the test stick, allowing esti-
control. Clay interactions, solubility mation of pH to 0.5 pH units over the
of various components and effective- entire pH range.
ness of additives are all dependent on Procedure
pH, as in control of acidic and sulfide 1. Place an indicator stick in the mud
corrosion processes. and allow it to remain until the color
Two methods are used for measuring has stabilized, usually less than a
the pH of freshwater drilling mud: a minute. Rinse the stick off with
modified colorimetric method, using deionized water but do not wipe.
plastic backed test strips (sticks); and 2. Compare the colors of the stick
the potentiometric method, employing with the color standard provided
the glass-electrode electronic pH meter. and estimate the pH of the mud.
The plastic strip method is frequently 3. Report the pH of the mud to the
used for field pH measurements, but is nearest 0.5 pH units.
not the preferred method. It is reliable
only in very simple water muds. Mud
solids, dissolved salts and chemicals,
and dark-colored fluids cause errors
in pH plastic strip values.
A) INDICATOR STICKS
Description
The “colorpHast pH indicator” sticks
(see Figure 11) are coated with indica-
Figure 11: pH indicator sticks.
tors of such nature that the color is

CHAPTER
3 Testing
B) PH METER 13. Clean electrodes-wash with

Description distilled water and blot dry.
The recommended method for pH 14. Place probe into pH 7.0 buffer
measurement of drilling fluid is with solution.
the glass-electrode electronic pH meter 15. Turn on meter, wait 60 sec for
similar to the Orion model No. 201. reading to stabilize. If meter read-
This meter is accurate and gives reli- ing does not stabilize, see cleaning
able pH values, being essentially free procedures.
of interferences. Measurements can 16. Measure temperature of pH 7.0
be made quickly and easily, automati- buffer solution.
cally adjusting slope and temperature 17. Set this temperature on
compensation. “temperature” knob.
18. Set meter reading to “7.0” using
Equipment
“calibration” knob.
1. pH meter (e.g. Orion 201). 19. Rinse and blot probe dry.
2. Glass pH electrode. 10. Repeat operations in Steps 6 through
3. Buffer solutions (4, 7 and 10 pH). 9 using pH 4.0 or 10.0 buffer. Use
4. Accessory equipment: pH 4.0 for low pH sample or pH
a. Soft-bristle brush. 10.0 for alkaline sample. Set meter
b. Mild liquid detergent. to “4.0” or “10.0” respectively, using
c. NaOH, 0.1 M, to recondition the “temperature” knob.
electrode. 11. Check the meter with pH 7.0 buffer
d. HCl, 0.1 M, to recondition again. If it has changed, reset to
electrode. “7.0” with “calibration” knob.
e. Distilled or deionized water. Repeat Steps 6 through 11. If
f. Soft tissues to blot electrodes. meter does not calibrate properly,
g. Glass thermometer, 32 to 212°F. recondition or replace electrodes
Procedure as given in cleaning procedures.
11. Obtain sample of fluid to be 12. If meter calibrates properly, rinse
tested and allow it to reach and blot dry the electrodes. Place
75±5°F (24±3°C). in sample to be tested. Allow about
12. Allow buffer solutions to also reach 60 sec for reading to stabilize.
the same temperature as the fluid to 13. Record measured pH along with
be tested. For accurate pH meas- the temperature of sample tested.
urement of the test fluid, buffer Indicate whether mud or filtrate
solution and reference electrode was tested.
must all be at the same tempera- 14. Carefully clean the electrodes in
ture. The pH of the buffer solution preparation for next usage. Place
indicated on the container label is in storage bottle with electrode
only at 75°F (24°C). If attempting through the cap. Use pH buffer 7.0
to calibrate at another tempera- to store the electrode. Deionized
ture, the actual pH of the buffer water is usually not desired to
at this temperature must be used. store the electrode. If it is not
Tables of the buffer pH values at used for a prolonged time remove
various temperatures are available any batteries.
from the supplier and should be 15. Turn meter off and close cover to
used in the calibration procedure. protect instrument.

CHAPTER
3 Testing
as indicated by slow response, drift-

ing of readings, or if “slope” and
“calibration” cannot be mutually set.
3. Recondition by soaking electrodes
for 10 min in 0.1 molar HCl fol-
lowed by rinsing in water and soak-
ing for 10 min in 0.1 molar NaOH
and rinsing again.
4. Check electrodes for response by
performing calibration steps.
Figure 12: Orion or suitable pH meter. 5. Only qualified individuals should
Cleaning procedures attempt this next step. If no response,
soak electrode for a maximum of
1. Cleaning the electrodes will be nec-
2 min in 10% NH4F•HF solution
essary periodically, especially if oil
(CAUTION: This is a strong and toxic
or clay particles coat the face of the
acid). Repeat calibration steps.
glass electrode or the porous face of
6. Replace electrode system if above
the reference electrode. Clean the
steps fail to recondition it.
electrodes with the soft-bristle
brush and mild detergent.
2. Reconditioning electrodes may be
necessary if plugging becomes severe,
Section 7. Chemical Analysis of Water-Base Drilling Fluids
A) ALKALINITY (Pf, Mf, Pm AND 1) PROCEDURE FOR FILTRATE ALKALINITY

LIME CONTENT) (Pf AND Mf)
Equipment 1. Measure 1-ml filtrate into the titra-
The following materials are required tion vessel, and add 5 ml deionized
to determine the alkalinity and lime water.
content of drilling fluids: 2. Add 2 or more drops of phenolph-
1. Standardized acid solution, 0.02 N thalein indicator. If the solution
(N/50); sulfuric or nitric acid (NOTE: turns pink.
Standardized 0.1N (N/10) acid solution 3. Add 0.02 N acid drop by drop from
may also be used, but it is converted to the pipette with stirring, until the
the equivalent ml 0.02 N by multiply- pink color just disappears. If the
ing by 5). sample is so colored that the color
2. Phenolphthalein indicator solution. change of the indicator is masked,
3. Methyl orange/brom cresol green the endpoint is taken when the pH
indicator solution. API recommends drops to 8.3, as measured with the
methyl orange (yellow to pink). glass electrode pH meter. (The sample
4. Titration vessel, 100 to 150 ml, can be diluted with distilled water.)
preferably white. 4. Report the phenolphthalein alkalin-
5. Graduated pipettes: one 1-ml and ity of the filtrate, Pf, as the number
one 10-ml. of ml of 0.02 N acid required per ml
6. Stirring rod. of filtrate to reach the end point.
7. One 1-ml syringe.
8. Glass-electrode pH meter (suggested).

CHAPTER
3 Testing
5. To the same sample used for mea- drops to 8.3 as measured with the
suring Pf, add 3 to 4 drops of methyl glass electrode.
orange/brom cresol green indicator; Report the phenolphthalein alkalinity
a green color will develop. of the mud, Pm, as the number of ml of
6. Titrate with 0.02 N acid until the 0.02 N (N/50) acid required per ml of
color changes to yellow. This will mud. If 0.1 N acid is used, Pm = 5 x
occur at pH of 4.3. ml of 0.1 N acid per ml mud.
7. The Mf is reported as the total ml
3) PROCEDURE FOR LIME CONTENT
of acid used for Pf plus this last
titration. Determine the Pf and Pm, as described
in the preceding paragraphs.
Example:
Determine the volume fraction of
If 0.5 ml acid was used to titrate the water in the mud, Fw (decimal fraction
phenolphthalein endpoint, the Pf is 0.5. of water), using the value from the
If an additional 0.3 ml acid was retort test.
used to titrate to the methyl orange Report the lime content of the
endpoint, the Mf is 0.8. mud in lb/bbl calculated from the
BaCl2 procedure: following equation:
1. Measure 1 ml of filtrate into a Lime (lb/bbl) = 0.26 x (Pm - FwPf).
titration vessel.
2. Add 2 drops of 10% barium chloride 4) FILTRATE ALKALINITY: P1 AND P2
solution (NOTE: BaCl2 is poisonous; Equipment
do not pipette with mouth). 11. Standard sulfuric acid solution,
3. Repeat Steps 2 through 4 for the 0.02 N (N/50).
Pf titration. 12. Sodium hydroxide solution,
4. As a rule of thumb, if the BaCl2 0.1 N (N/10).
PAlkalinity is one-half or less than 13. Barium chloride solution, 10%.
the previous Pf titration, carbonate 14. Phenolphthalein Indicator.
contamination exists. 15. Deionized water.
Example: 16. pH strips or glass electrode
If 1 ml acid was used to titrate to the pH meter.
endpoint for Pf, the Pf is 1.0. 17. Titration vessel, 100 to 150 ml,
If 0.4 ml acid was used to titrate to preferably white.
the PAlkalinity endpoint with BaCl2, the 18. Pipette: one 1-ml, one 2-ml and
BaCl2 value is 0.5. Thus, carbonate con- one 10-ml.
tamination exists because the BaCl2 is 19. Graduated cylinders: one 25-ml
less than one-half the Pf. and one 5- or 10-ml.
10. Stirring rod.
2) PROCEDURE FOR MUD ALKALINITY (Pm)
Procedure: P1 - P2
Measure 1 ml of mud into the titration 1. Measure 1 ml of filtrate into the
vessel using the syringe. Dilute the titration vessel and add 24 ml of
mud sample with 25 ml of distilled deionized water.
water. Add 5 drops of phenolph- 2. Add 2 ml of 0.1 N sodium hydrox-
thalein indicator and, while stirring, ide and stir well. Measure the pH
titrate quickly with 0.02 N acid or 0.1 with the pH strip or pH meter. If
N acid until the pink color disappears. the pH is 11.4 or greater, proceed
If the sample is so colored that the to the next step. If the pH is less
color change of the indicator is masked, than 11.4, add another 2 ml of
the end point is taken when the pH 0.1 N sodium hydroxide.

CHAPTER
3 Testing
3. Using the graduated cylinder, mea- CO2 present, but it is also sensitive to
sure 2 ml of barium chloride and the flow rate and the total gas volume
add to the titration vessel. Add 2 passed through the tube. Therefore, for
to 4 drops of phenolphthalein more accurate results, the gas exiting
with stirring. the gas train must first be captured in
NOTE: Do not use your mouth to a 1-l bag to allow the CO2 to mix uni-
pipette; the barium chloride solution formly with the carrier gas. The CO2
is poisonous. Dräger tubes are very sensitive to incor-
4. Immediately titrate the mixture rect use. The filtrate must be free of
with standard sulfuric acid to the solids. Therefore, the first spurt of the
first disappearance of the pink color filtrate should be discarded, because it
(or to pH 8.3 with the pH meter). may contain CaCO3 particles that can
The color may reappear after a short cause errors on the high side. The con-
time; do not continue the titration. tents of the bag are passed from the bag
5. Report the alkalinity, P1, as the through the Dräger tube using 10 strokes
ml of 0.02 N sulfuric acid required of the Dräger hand pump. This tech-
to titrate to the phenolphthalein nique will draw exactly 1 l of gas
endpoint. through the tube.
Procedure: P2 (blank) Equipment
1. Omit the filtrate, but otherwise 11. Deionized water.
repeat the procedure for P1, using 12. Octyl alcohol defoamer.
exactly the same quantities of water 13. Sulfuric acid, approximately 5 N,
and reagents. Titrate using the same reagent grade.
procedures as for P1. 14. Garrett Gas Train apparatus.
2. Report the alkalinity, P2, as the 15. Dräger CO2 analysis tube, “CO2
ml of 0.02 N sulfuric acid required 100/a” labeled 100 to 3,000 ppm.
to titrate to the phenolphthalein Factor = 2.5 (be sure to check to
end point. see if the factor has changed).
Calculations 16. Dräger 1-l bag, #762425.
17. Dräger “Multigas Detector” hand
Within limitations, the various ionic
vacuum pump.
alkalinities can be calculated as follows:
18. Glass stopcock, 8 mm, 2-way bore.
When P1 > P2 19. Hypodermic syringes: one 10-ml
OH– (mg/l) = 340 x (P1 – P2) with 21 gauge needle (for acid), one
CO32– (mg/l) = 1,200 x [Pf – (P1 – P2)] 10-ml, one 5-ml and one 2.5-ml.
When P1 < P2 10. N2O gas cartridges (e.g. Whippets).
HCO3– (mg/l) = 1,220 x (P2 – P1) Bottled nitrogen or helium gas can
CO32– (mg/l) = 1,200 x Pf also be used. Do not use Whippets
B) GARRETT GAS TRAIN (GGT) TEST in any other test.
FOR CARBONATES Procedure
Purpose 11. Be sure the gas train is clean, dry
This procedure uses the Garrett Gas and on a level surface.
Train, analyzing the soluble carbonates 12. With the regulator backed off,
on a filtrate sample of water-base drill- install and puncture a N2O car-
ing fluid. The CO2 Dräger tube responds tridge. Do not use compressed
to the CO2 gas passing through it by air or a CO2 cartridge.
turning purple. The stain length is 13. Add 20 ml deionized water to
primarily sensitive to the amount of Chamber 1.

CHAPTER
3 Testing
Attach Dräger hand pump to other

end of Dräger tube.
12. Open stopcock on bag. With hand
pressure, fully depress the hand
pump, then release so that gas
flows out of the bag and through
the Dräger tube. Operate the hand
pump 10 strokes, which should
essentially empty the gas bag.
13. Observing a purple stain on the
Dräger tube means CO2 was pre-
Figure 13: Garrett Gas Train.
sent in the gas bag. Record the
14. Add 5 drops of defoamer to stain length in units marked on
Chamber 1. the Dräger tube.
15. Install the top on the gas train 1) DRÄGER TUBE IDENTIFICATION
and hand-tighten evenly to seal
all O-rings. 1 2 3
Carbonate Sample Dräger 4
16. Attach the flexible tubing from the Range Volume Tube Tube
regulator onto the dispersion tube (mg/l) (ml) Identification Factor
of Chamber 1. 25 - 750 10 CO2 100/a 2.5*
17. Inject with syringe an accurately 50 - 1,500 5 CO2 100/a 2.5*
measured sample of filtrate into 100 - 3,000 2.5 CO2 100/a 2.5*
Chamber 1, (see Figure 13). Flow 250 - 7,500 1 CO2 100/a 2.5*
*NOTE: Tube factor “2.5” applies to new tubes, CO2 100/a (cat. no.
carrier gas through train for 1 min 8101811) with scale 100 to 3,000. Old tubes use tube factor 25,000
to purge air from system. Stop gas with scale 0.01 to 0.3%.
flow. Table 3: Sample volumes and tube factor

18. Install one end of a piece of flexible to be used for various carbonate ranges.
tubing into the stopcock which is
Calculations
fitted directly into the gas bag. Have
the gas bag fully collapsed. Fit the Using the measured sample volume,
other end of the tubing onto the the Dräger tube’s purple stain length
outlet tube of Chamber 3. and tube factor or 2.5 (see Table 3),
19. Slowly inject 10 ml sulfuric acid calculate the soluble carbonates in the
into Chamber 1 through the rub- filtrate sample using the following
ber septum using the hypodermic equation:
syringe and needle. Gently shake tube stain length x 2.5
CO2– (mg/l) =
the gas train to mix acid with ml of sample filtrate
sample in Chamber 1. NOTE: The gas train apparatus MUST be
10. Open the stopcock on the gas bag. cleaned after each use or the acid used
Restart N2O flow gently and allow will cause severe damage to the equip-
gas bag to fill. When bag is full do ment. To clean the gas train, remove the
not burst it, shut off N2O flow and flexible tubing and remove the top. Wash
close the stopcock. Immediately out the chambers with warm water and
proceed to Step 11. mild detergent, using a brush. Use a pipe
11. Remove the tubing from Chamber 3 cleaner to clean the passages between
outlet and re-install it onto the chambers. Wash, rinse and then blow out
upstream end of the CO2 Dräger the dispersion tubes with air or N2O gas.
tube after breaking off the ends of Rinse the unit with deionized water and
the Dräger tube (observe that the allow to drain dry. Do not use the Nitrous
arrow indicates gas flow direction). oxide for any other test, or as a gas source.
CHAPTER
3 Testing
It can cause an explosion if misused in

other applications. (NEVER use them as 300
200
a gas source for High-Temperature, High- 150
Pressure (HTHP) cell or filtration — only 100
GGT for carbonates.)
Salt (mg/l x 1,000)

50
–
40
C) CHLORIDE (Cl ) 30
20
Purpose
The salt, or chloride, test is very sig- 10
nificant in areas where salt can conta- 5

minate the drilling fluid. This would 4
3
include the majority of the world’s 2
oilfields. The salt may come from 1
makeup water, sacks, stringers, beds .1 .2 .3.4.5 1 2 3 4 5 10 15 20 30
or saltwater flows. Salt (% by weight)
Equipment Figure 14: Salt milligrams per liter vs.

The following materials are required salt percent by weight.
to determine the chloride ion concen-
tration in the mud filtrate. nitrate solution are used, consider
1. Silver nitrate solution, 0.0282N or repeating the test with a smaller,
0.282N (strong) AgNO3, stored in accurately measured sample of filtrate
an amber or opaque bottle. or use a dilution with factor.)
2. Potassium chromate indicator Calculations
solution. If the chloride ion concentration of
3. Acid solution 0.02 N sulfuric or the filtrate is less than 10,000 mg/l,
nitric acid. use the 0.0282 N silver nitrate solu-
4. Distilled water. tion equivalent to 0.001 g Cl– ion
5. Two graduated pipettes: one 1-ml per ml.
and one 10-ml. Report the chloride ion concentra-
6. Titration vessel, 100 to150 ml, tion of the filtrate in milligrams per
preferably white. liter, calculated as follows:
7. Stirring rod. Cl– (mg/l) =
Procedure ml of 0.0282 N silver nitrate x 1,000
1. Measure 1 or 2 ml of filtrate into a ml of filtrate
titration vessel.
2. Add the amount of acid required in If the chloride ion concentration of
the Pf titration. the filtrate is greater than 10,000 mg/l,
3. Add 25 ml of distilled water and use the 0.282 N silver nitrate (equivalent
10 drops of potassium chromate to 0.01 g Cl– ion per ml). Report the
solution. Stir continuously and titrate chloride concentration of the filtrate in
with standard silver nitrate solution mg/l, calculated as follows:
drop by drop from the pipette, until Cl– (mg/l) =
the color changes from yellow to ml of 0.282 N silver nitrate x 10,000
orange-red and persists for 30 sec. ml of filtrate
4. Record the number of ml of silver For any normality silver nitrate:
nitrate required to reach the end-
N x 35,000 x ml used
point. (If over 10 ml of 0.282N silver Cl– (mg/l) =
ml of filtrate sample

CHAPTER
3 Testing
D) CALCIUM - QUALITATIVE E) TOTAL HARDNESS

Purpose 1) CALCIUM AND MAGNESIUM TOGETHER
Water containing a large amount of dis-
solved calcium and magnesium salts is QUANTITATIVE
referred to as “hard water.” The com- Equipment
mon evidence of hardness in water at 11. EDTA (Standard Versenate) solu-
home is the difficulty of producing a tion 0.01 M (1 ml = 400 mg Ca2+
lather with soap. In many oil fields, the or 1,000 mg CaCO3).
water available for use is quite hard. 12. Strong buffer solution (ammonium
Drilling clays have low yields when hydroxide/ammonium chloride).
mixed in hard water. The harder the 13. Calmagite Indicator solution.
water, the more bentonite it takes to 14. Titration dish, 100 to 150 ml,
make a satisfactory gel mud. In extreme preferably white.
cases it has been found economical to 15. Three graduated pipettes: one
treat the water chemically before using 1-ml, one 5-ml and one 10-ml.
it for mixing mud, but it is not gener- 16. Graduated cylinder, 50 ml.
ally economical to do this. Frequently, 17. Distilled water.
however, where there is a choice of two 18. Stirring rod.
or more sources of water for the rig, it 19. 8N NaOH or KOH solution.
may be desirable to make a simple test 10. Calcon Indicator or Calver II.
to select the softer of the two. 11. Porcelain spoon/spatula.
Field engineers are familiar with the 12. Masking Agent: 1:1:2 mixture vol-
effects on the mud when anhydrite ume triethanolamine: tetraethyl-
(calcium sulfate) or gyp formations are enepentamine: water (API).
drilled. Calcium may be picked up in Determining the total hardness of
drilling cement plugs and sometimes water or mud filtrate can be done by
in penetrating sections of limey shale. performing Part A as shown. This test
Any extensive calcium contamination is performed to obtain the ppm total
can result in high water loss and high hardness reported as calcium for the
gels. The detrimental effect of cement mud report form.
on increased Pm is due to the high It may be required to determine the
alkalinity (lime) content. concentration of magnesium as well as
Equipment calcium. In this case, use the procedure
The following materials are required described in 2) CALCIUM AND MAGNESIUM
to qualitatively determine the pres- SEPARATELY. This measures calcium specifi-
ence of calcium and/or magnesium. cally, rather than reporting the Mg2+ as
1. Test tube. Ca2+. After the calcium is known, the
2. Dropper bottle of saturated solution magnesium concentration is calculated
of ammonium oxalate. from the difference in the two titrations.
Procedure Caustic soda (called “calcium buffer
solution” here) precipitates the magne-
Place 1 to 3 ml of filtrate in test tube.
sium as the hydroxide, and the calcium
Add a few drops of saturated ammo-
is titrated with an indicator that is
nium oxalate. The formation of a
specific for calcium.
white precipitate indicates the pres-
ence of calcium. Record as light, Procedure (total hardness as Ca2+)
medium or heavy. 1. Add approximately 20 ml of distilled
water to titration vessel.
2. Add 1 ml of the water or filtrate to
be tested.

CHAPTER
3 Testing
3. Add 1 ml of strong buffer solution 2) CALCIUM AND MAGNESIUM SEPARATELY

(NH4OH base). 1. Add approximately 20 ml of distilled
4. Add about 6 drops of Calmagite water to the titration vessel.
and mix with a stirring rod. A wine 2. Add the same amount of water or
red color will develop if calcium filtrate to be tested as performed in
and/or magnesium is present. the previous hardness test.
5. Using a pipette, titrate with 3. Add 1 ml Masking Agent.
Standard Versenate Solution, stir- 4. Add 1 ml of 8N NaOH or KOH and 1⁄4
ring continuously, until the sample porcelain spoonful (0.2 g) of Calcon
first turns to blue with no undertint Indicator and mix with a stirring rod.
of red remaining. Record the num- 5. Titrate with Standard Versenate solu-
ber of ml of Standard Versenate tion until the indicator turns from
solution used. (If magnesium is to wine red to blue with no undertint of
be measured as in Procedure 2, red remaining. Record the number of
record this value as “A” ml.) ml of Standard Versenate required
Calculations (record this value as “B” ml).
Total hardness as Ca2+ (mg/l) = Calculations
ml of Standard Versenate x 400 B x 400
Calcium (mg/l) =
ml of sample ml of sample
CaCO3 (mg/l) = (A – B) x 243
ml of Standard Versenate x 1,000 Magnesium (mg/l) =
ml of sample
ml of sample
F) HARDNESS IN DARK FILTRATES
Occasionally in dark-colored filtrate,
it is difficult to see the endpoint to 1) TOTAL HARDNESS IN DARK FILTRATES
determine total hardness. The follow- QUANTITATIVE

ing method can be used to better Purpose
observe the endpoint. Calculations
Occasionally there is difficulty in accu-
remain the same.
rately titrating for hardness concentra-
1. Add approximately 20 ml of distilled
tion in dark-colored filtrates due to the
water to titration vessel.
subtle change in color of the filtrate
2. Add 1 ml filtrate to titration dish
when the endpoint is reached. Thus,
(0.5 ml accurately measured can be
the following method has been devel-
used if the endpoint cannot be seen
oped and is recommended only when
with a 1 ml sample).
the previous hardness test procedure
3. Add 1 ml Masking Agent.
becomes difficult or impossible.
4. Add 1 ml of strong buffer solution.
5. Add 6 drops Calmagite Indicator Equipment
and stir. 11. Acetic acid: glacial (caution).
6. Using a pipette, titrate with Standard 12. Calcon or Calver II Indicator
Versenate solution until the color (specific for Ca2+).
changes to blue/green. Record the 13. Sodium hypochlorite 5.25%
number of ml used and calculate (CloroxT).
the same as before. 14. Calmagite Indicator.
15. Sodium hydroxide; 8N NaOH.
Calculations
16. Masking Agent.
Total hardness as CaCO3 (mg/l) =
17. Standard Versenate solution
ml of Standard Versenate x 1,000
0.01 Molar.
ml of sample
18. Strong buffer solution.

CHAPTER
3 Testing
19. Beaker, 100-ml. 3. Add 1 ml of acetic acid and mix.

10. Graduated cylinders, two 10-ml. 4. Heat to boiling and boil for
12. Graduated pipette, 10-ml. 5 min. Maintain volume by
13. Hot plate. adding deionized water.
14. Volumetric pipette, 1-ml. 5. Remove the beaker from the hot
15. Porcelain spoon/spatula for solid plate and let it cool to room tem-
indicator addition. perature. Wash down the sides of
Method I (includes all metals which the beaker with deionized water.
are titrated by Versenate solution) 6. Add 1 ml of strong buffer solution
CAUTION: Work in well-ventilated area. and swirl to mix.
Do not breathe fumes. 7. Add 1 ml of Masking Agent and mix.
1. Using a 1-ml volumetric pipette, 8. Add 6 drops of Calmagite and mix.
transfer 1 ml of filtrate to a A wine red color will develop if cal-
100-ml beaker. cium and/or magnesium is present.
2. Add 10 ml Clorox (be sure it is fresh 9. Using a pipette, titrate with Standard
as it will deteriorate with time). Versenate, stirring continuously,
Swirl to mix. until the sample turns blue with no
3. Add 1 ml of acetic acid and swirl undertint of red remaining. Record
to mix. the number of ml of Standard
4. Heat to boiling on high heat and Versenate used. This is Value A.
boil for 5 min. Maintain volume Calculations
by adding deionized water. Total hardness as Ca2+ (mg/l) = A x 400
5. Remove the beaker from the hot
2) CALCIUM AND MAGNESIUM SEPARATELY
plate and let it cool to room tem-
perature. Wash down sides of the 1. Using a 1-ml volumetric pipette,
beaker with deionized water. transfer 1 ml of filtrate to a 100-ml
6. Add 1 ml strong buffer solution and Pyrex beaker.
swirl to mix. 2. Add 10 ml Clorox and swirl to mix.
7. Add 6 drops of Calmagite and mix. 3. Add 1 ml acetic acid and mix.
A wine red color will develop if 4. Heat to boiling and boil for
hardness is present. 5 min. Maintain volume by
8. Using a pipette, titrate with Standard adding deionized water.
Versenate solution, stirring continu- 5. Remove the beaker from the hot
ously, until the sample turns to blue plate and let it cool to room tem-
with no undertint of red remaining. perature. Wash down the side of
The color change will be purple to the beaker with deionized water.
slate gray with dark filtrates. Record 6. Add 1 ml calcium buffer (sodium
the number of ml Standard hydroxide) and mix (precipitates
Versenate solution used. Mg2+).
7. Add 1 ml Masking Agent and mix.
Calculations
8. Add 1⁄4 spoonful (0.2 g) of Calcon
Total hardness as Ca2+ (mg/l) = Indicator and mix. A wine red color
ml Standard Versenate x 400 will develop if calcium is present.
Method II (includes calcium and 9. Titrate with Standard Versenate
magnesium reported as Ca2+) until the indicator turns from wine
1. Using a 1-ml volumetric pipette, red to blue with no under tint of
transfer 1 ml of filtrate to a 100-ml red remaining. Record the number
PyrexT beaker. of ml Standard Versenate required.
2. Add 10 ml Clorox (be sure Clorox is This is Value B.
fresh). Swirl to mix.

CHAPTER
3 Testing
Calculations 13. Calmagite Indicator.

Calcium (mg/l) = B x 400 14. Standard Versenate solution
Magnesium (mg/l) = (A - B) x 243 0.01 Molar.
15. Strong buffer solution.
G) SULFATE
16. Beaker, 400-ml.
1) QUALITATIVE 17. Calibrated beaker at 250 ml
Purpose volume mark.
The sulfate ion is present in many nat- 18. Hot plate.
ural waters due to the solvent action 19. Pipettes: 1-ml, 2-ml and 10-ml.
of water on the minerals in the earth. 5-ml syringe.
Anhydrite (calcium sulfate) is a slightly 10. Titration vessel, 100- to 150-ml,
soluble contaminant encountered in preferably white.
drilling in certain areas. Frequently it 11. Mud still (retort).
is desirable to know the sulfate ion Procedure
content in the filtrate. Sulfate ion con- 11. Add 5 ml of mud to calibrated
centrations around 2,000 mg/l could beaker, then add 245 ml water
contribute to high viscosity and to make final volume at 250-ml
fluid-loss control problems. calibration mark.
Equipment 12. Heat to 160°F and stir for about
15 to 20 min. Stir while heating if
The following materials are required
possible. (If there are no heating
to qualitatively determine the pres-
facilities available, stir for 30 min.)
ence of sulfate:
13. Cool with stirring and make up
1. Test tube.
the volume to exactly 250 ml with
2. Dropper bottle of 10% barium chlo-
water using the calibrated container.
ride solution. (POISON. Do not pipette
14. Filter with the filter press, discard-
by mouth.)
ing first cloudy portion of filtrate,
3. Dropper bottle of strong nitric acid.
and retain only clear filtrate.
Procedure 15. To 10 ml of filtrate add 1 ml of
Place about 3 ml of filtrate in a test Strong Buffer and 6 drops of
tube. Add a few drops of barium chlo- Calmagite Indicator.
ride solution. The formation of a white 16. Titrate with Standard Versenate
precipitate indicates the presence of solution, stirring continuously
sulfates and/or carbonates. Add a few until sample turns blue (or green
drops of concentrated nitric acid. If the for dark-colored filtrate) with no
precipitate dissolves, it is carbonate; if undertint of red remaining. Record
not, it is sulfate. Record the amount of the number of ml Standard
precipitate remaining after the acid Versenate solution used (Vt).
treatment as light, medium or heavy. 17. Clean the titration vessel and add
2) AVAILABLE (UNREACTED) CALCIUM SULFATE
approximately 20 ml water.
18. Add 1 ml of filtrate from the mud.
Purpose
19. Add 1 ml of Strong Buffer solution.
When running gyp muds it is necessary 10. Add 1 ml of Masking Agent.
to know how much available gyp (cal- 11. Add 6 drops of Calmagite and mix
cium sulfate) is available in the system. with a stirring rod.
Equipment 12. Titrate with Standard Versenate
11. Masking Agent: 1:1:2 mixture solution, stirring continuously until
by volume of triethanolamine: sample turns to blue (or green for
tetraethylenepentamine: water. dark-colored filtrate) with no
12. Deionized water. undertint of red remaining.

CHAPTER
3 Testing
13. Record the number of ml of to determine sample size. Be sure to

Standard Versenate solution use a pipette to measure the amount
used (Vf). of filtrate and/or diluted sample.
Calculations 2. Add 4 ml of NaOH with a 5-ml
Available CaSO4 (lb/bbl) = pipette, 25 ml of STPB solution
2.38 x Vt – [0.2 x (Fw x Vf)] measured with a 25-ml graduate
and enough deionized water to
Where:
bring the level of the solution up
Vt = Number of ml Standard Versenate
to the 100-ml mark.
solution used to titrate 10 ml of
3. Mix and allow to stand 10 min.
clear filtrate in Step 6.
4. Filter into a clean 100-ml graduated
Vf = Number of ml Standard Versenate
cylinder. If the filtrate is cloudy, the
solution used to titrate 1 ml of
solution must be refiltered.
mud filtrate in Step 13.
5. Transfer 25 ml of clear filtrate (mea-
Fw = Freshwater fraction of mud
sured with a 25-ml cylinder) into a
obtained with mud still. Water
250-ml beaker.
%/100 = Fw.
6. Add 15 drops of bromophenol blue
H) POTASSIUM (K+) indicator.
When it is necessary to determine the 7. Titrate with QAS solution until color
potassium ion concentration, either of changes from purple-blue to light-
the following procedures can be used blue. Record ml of QAS solution
effectively. Procedure I may be accu- used. Continue titration to 25 ml to
rately used for any concentration of ensure end point has been reached
potassium ion. Procedure II is a quick and no purple-blue color remains. If
method, used for high concentrations possible, use magnetic stirrer with
of potassium. light. Do not use a titration dish.
1) PROCEDURE I — POTASSIUM BELOW Ratio of QAS to STPB = ml QAS ÷ 2
5,000 mg/l (STPB METHOD) If ratio is other than 4.0±0.05, it
Equipment must be used as a correction factor in
1. Standard Sodium Tetraphenyl the calculation of mg/l K+.
Borate (STPB) solution. Calculations
2. Quaternary Ammonium Salt (QAS)
(25 – ml of QAS) x 1,000
solution, hexadecyltrimethyl K+ (mg/l) =
ammonium bromide. ml of filtrate
3. Sodium hydroxide (NaOH) solution If correction factor is necessary:
(20%); 20 g/80 ml deionized water. K (mg/l) =
+
4. Bromophenol blue indicator. ml of QAS x 4

5. Serological (graduated) pipettes:
one 2-ml in 0.1-ml subdivisions,
[ (
25 –
ratio of QAS to STPB )]
x 1,000
two 5-ml and two 10-ml. ml of filtrate*

6. Graduated cylinders: two 25-ml and * For calculation, use ml filtrate from
two 100-ml. Procedure No. 1, labeled ml filtrate *
7. Funnel: 100-ml. (calculations). This procedure is called a
8. Filter paper. back titration. Step 2 precipitates the
9. Beakers: two 250-ml and deionized potassium from solution. The potassium
water. ion is filtered out in Step 4. Titration
Procedure with the QAS solution determines the
1. Place the proper amount of filtrate amount of unreacted STPB solution.
into a 100-ml graduate, using Table 4

CHAPTER
3 Testing
2) PROCEDURE II — POTASSIUM ION (SODIUM slowly turn the crank and

PERCHLORATE METHOD) count the number of revolu-
Equipment tions of the rotor head during
1. Standard sodium perchlorate solution: one turn of the crank.
150.0 g NaClO4 per 100 ml distilled 2. Determine the number of crank
water. turns it takes to get 1,800 revo-
NOTE: Sodium perchlorate is explo- lutions of the rotor head.
sive in the dry state, if heated to a 3. To maintain a constant speed
high temperature or allowed to contact for 1 min, take the required
organic reducing agents. The perchlo- number of crank turns and
rate is not hazardous if kept water divide by 12. This will give the
wet. They will decompose harmlessly number of crank turns needed
if dispersed in a bucket of water and per 5 sec.
then disposed of properly. 4. Now, look at the second hand
2. Standard potassium chloride solu- of your watch. Start cranking
tion, 14.0 g KCl made up to 100 ml rapidly and count the number
with distilled water. of crank turns in 5 sec. If the
3. 10 ml clinical centrifuge tubes, number is greater than 10, slow
Kolmer-type only; Corning 8360. down a little and count turns
4. Centrifuge, horizontal-swing rotor for another 5 sec. Continue
head (manual or electrical) capable of adjusting your speed until the
producing approximately 1,800 RPM. required number of turns is
5. Standard calibration curve for achieved and becomes natural.
potassium chloride. 2. Preparation of standard calibration
Preparation curve for potassium chloride (see
1. Calibrate the centrifuge. Figure 15 or use the following to
a. If electrical centrifuge is used, prepare curve).
calibrate to 1,800 RPM using a. Prepare standards over the range of
rheostat. 1 to 8% KCl by adding appropriate
b. If manual centrifuge is used, ml of standard potassium chloride
fairly constant 1,800 RPM can solution (0.5 ml for each 3.5 lb/bbl)
be obtained as follows: to centrifuge tube and dilute to
1. Determine the number of revo- 7 ml with distilled water.
lutions of the rotor per each b. Add 3 ml of sodium perchlorate
turn of the crank; i.e., very solution to each tube.
Estimated ppm K+ Sample Preparation Filtrate (ml)

Over 100,000 Take 1 ml filtrate, add 9 ml distilled water.
Mix and use 1 ml solution for sample. 0.10
50,000 - 100,000 Take 1 ml filtrate, add 9 ml distilled water.
20,000 - 50,000 Take 1 ml filtrate, add 9 ml distilled water.
10,000 - 20,000 Take 1 ml undiluted filtrate. 1.00
250 - 2,000 Take 10 ml undiluted filtrate. 10.00
NOTE: It is important to check the concentration of QAS solution vs. the STPB solution at monthly intervals. To determine the equivalent QAS, dilute
2 ml of the STPB solution in titration vessel with 50 ml distilled water. Add 1 ml sodium hydroxide solution and 10 to 20 drops of the bromophenol
blue indicator. Titrate with the QAS solution until the color changes from purple-blue to light-blue.
Table 4: Potassium sample sizes.

CHAPTER
3 Testing
c. Centrifuge for 1 min at 1,800 RPM 1.40

Example plot
and read the precipitate volume 1.30
(construct a similar
1.20
immediately. calibration curve for
1.10 actual chemicals)
d. Rinse tubes and dispose of the 1.00
Precipitate (ml)
liquid properly. 0.90
0.80
e. Plot ml of precipitate vs. potas- 0.70
sium chloride content (lb/bbl) 0.60
Dilute sample
on rectangular graph. 0.50
volume to
0.40
Procedure * keep test result
0.30
<21 lb/bbl.
1. Measure 7 ml of filtrate into cen- 0.20
0.10
trifuge tube. Add 3 ml of the sodium 0.00
1 lb/bbl = 2.853 kg/m3
perchlorate solution to the tube (if 0 3.5 7.0 10.5 14.0 17.5 21.0 24.5 28.0
potassium is present, precipitation KCl concentration (lb/bbl)
*Not valid for KCl concentrations
occurs at once). DO NOT AGITATE! below 3.5 lb/bbl
Centrifuge at constant speed, approx-
imately 1,800 RPM for 1 min and Figure 15: KCl concentration calibration curve.
read the precipitate volume immedi-
ately. Rinse the precipitate from the distilled water and agitated before
tube into a bucket of water. adding the sodium perchlorate solu-
NOTE: To ensure all potassium has tion. If filtrate volumes other than
been removed, add 2 to 3 drops of the 7 ml are used, the KCl concentration
sodium perchlorate to the centrifuge should be calculated as follows:
tube after centrifuging. If a precipitate is KCl (lb/bbl) =
formed, the total amount of potassium 7
(value from standard curve)
ion was not measured; sample must be ml of filtrate
diluted as in Note 2. This method was developed as a field
2. Determine the potassium chloride procedure and should be used in that
concentration by comparing the respect. It is to aid in maintaining the
precipitate volume measured with potassium ion in the mud filtrate at or
the standard curve (see Figure 15). above a certain level. It can best be used
3. Report the potassium concentration when potassium ion concentration is
as lb/bbl KCl or kg/m3. above 5,000.
Calculations
The potassium concentration may also I) NITRATE ION CONCENTRATION
be reported as a weight % of KCl. Purpose

lb/bbl Fluids recovered from DST/formation
KCl (wt %) = tests are often difficult to identify as
3.5
being either filtrate or connate water.
lb/bbl x 2.853 = kg/m3 The use of the nitrate ion in the mud
K+ (mg/l) = 1,500 x KCl (lb/bbl) filtrate as a tracer permits a better
evaluation to be made.
NOTE 2: These two calculations
Equipment
assume a filtrate specific gravity of 1.00.
If the concentration of KCl exceeds Nitrate Test Kit (A.J. Chemical) plus
21 lb/bbl, the accuracy can be improved tablespoon for measuring lime.
by performing an appropriate dilution Procedure
to keep the test result in the 3.5 to 11. Measure a 5-ml sample of near col-
21 lb/bbl range. The volume in the orless filtrate into a test tube. If
tube should be made up to 7 ml with the filtrate is dark, the color must

CHAPTER
3 Testing
be removed by either dilution or 18. Prepare a blank by taking a 5-ml sam-

lime treatment (see Note 1 and ple which is treated identically to the
Table 3). sample in Step 1 with respect to
12. Add contents of a NO3-11 ampoule dilution and lime treatment, and
and shake for 3 min. add 5 ml of deionized water to
13. Let settle and decant liquid into a give the same dilution as indicated
second test tube. in Step 6.
14. Add contents of a NO3-12 ampoule 19. Place the colored unknown in the
to the decanted liquid in the second right hole of the comparator box.
test tube. 10. Place the blank in the left hole of
15. Shake and let stand in rack for the comparator box.
10 min for full color development. 11. While looking through the holes,
16. After full color development, rotate the wheel slowly until color
pour sample into a 10-ml gradu- intensities match. If sample color
ate and add deionized water to is darker than wheel color at 80
make the volume up to 10 ml. (see Note 2), estimate the dilution
Mix thoroughly. needed (see Table 5) to reduce
17. Transfer sample back to the second nitrate ion concentration to within
test tube. color wheel range and repeat test.
12. Record the dial reading.
Calculations
Clear filtrates:
dial reading x dilution factor
mg/l NO3– =
10
Colored filtrate requiring one lime treatment:
mg/l NO3– = – (6 x mg/1 NO3– in lime*)
10
Colored filtrate requiring two lime treatments:
mg/l NO3– = – 1 – (42 x mg/l NO3– in lime*)
10
*This value is marked on the lime container.
NOTE 1: The 5-ml sample taken at Step 1 does not have to be absolutely color-
less. A slight color can be tolerated if the proper blank is used as specified in
Step 8. Quite often the color is reduced to a satisfactory level by the dilution
that may be required to lower the NO3– concentration so it will fall within the
range of the color wheel at Step 11. An extremely dark filtrate, however, will
have to be decolorized. This is accomplished by diluting 5 ml of filtrate with
deionized water, adding 1 tablespoon of calcium hydroxide, shaking well and
then filtering with funnel. This gives an initial dilution factor of 6. If the fil-
trate is too dark, take 1 ml and dilute to 5 ml with deionized water to see if this
would be a satisfactory sample to use as Step 1. If not take 5 ml and repeat the
above dilution and treatment, and then filter again. This will give a dilution
factor of 36. No further decolorization should be necessary; however, further
dilution with deionized water may be necessary (see Table 5). But this may
not be known until completion of Step 11.
NOTE 2: The readings above 80 on the color wheel give erroneous results.
Therefore, samples having readings above 80 should be diluted and rerun.

CHAPTER
3 Testing
Dilution tables 13. Distilled water.

This table is to aid in selecting the 14. Boric acid solution, 2% by weight.
proper dilution of the original filtrate 15. Methyl Red Indicator.
(no lime treatment) or the additional 16. 6 N sodium hydroxide solution.
dilution after lime treatment, if the 17. 2 to 3 ft of 0.25-in. ID Tygon tubing.
approximate NO3– concentration of 18. No. 6 rubber stopper with a
original mud filtrates is known. Dilution 0.25-in. hole.
Factors (DF) for use in calculations are 19. 0.02 N sulfuric acid solution.
also shown. 10. Silicone defoamer (i.e. Dow-
Corning 84 AFC-78).
No lime treatment. 11. 0.25-in. OD glass tubing —
–
NO3 Dilution Dilution fire polished (2 pieces about
(mg/l) (ml) Factor
3 to 4 in. long).
0-8 None 1
8 - 20 2-5 2.5 Procedure
20 - 40 1-5 5 1. Attach the two pieces of glass tub-
40 - 80 1 - 10 10 ing to each end of the Tygon tub-
80 - 200 1 - 25 25 ing. Insert one end into the rubber
200 - 500 1 - 50 50 stopper so the end of the tube is
exactly flush with the bottom of
One lime treatment. the stopper.
Dilution Dilution 2. To one Erlenmeyer flask, add 25 ml
mg/l (ml) Factor
of the boric acid solution, and 6 drops
0 - 20 None 6
of Methyl Red Indicator. This is the
20 - 100 2-5 15
100 - 200 1-5 30
collection flask. Note the original
200 - 450 1 - 10 60
color which should be pink/red,
but not yellow.
Two lime treatments. 3. To the other Erlenmeyer flask (this
Dilution Dilution
is the reaction flask) add 50 ml
mg/l (ml) Factor distilled water, 2 ml of silicone
0 - 120 None 36 defoamer and 10 ml whole mud.
120 - 550 2-5 90 If the active POLY-PLUST concentra-
Table 5. tion is more than 1.5 lb/bbl, or if
the liquid POLY-PLUST is more than
The dilution factor column indicates 4.5 lb/bbl, use 5 ml whole mud,
the amount of filtrate used and the then double the result.
final volume to which it is diluted 4. Place the reaction flask containing
with deionized water. the mud on the hot plate and begin
J) PHPA POLYMER CONCENTRATION stirring. Add 3 ml of the 6 N sodium
Purpose hydroxide solution and immediately
fit the flask with the rubber stopper.
PHPA polymers are mud additives
5. Submerge the other end of the tub-
which help stabilize shales in a well-
ing (Pasteur pipette, if used) into the
bore. The following analysis will deter-
2% boric acid/methyl red solution.
mine the free polymer available to
6. Heat for 45 to 60 min, allowing a
adsorb on the wall of the hole.
gentle boiling. Approximately 25 ml
Equipment should condense in the collection
11. Hot plate/magnetic stirrer with flask during this time, with a color
magnetic stir bars. change from pink to yellow.
12. Two, 125-ml Erlenmeyer flasks.

CHAPTER
3 Testing
7. Adjust heat for neither too hot, nor 3. If the mud foams or boils over, use
cool enough to allow fluid to be more defoamer. Try to estimate the
pulled back. If the heat from the hot range of the active polymer so the
plate cycles from on to off, the cool- proper amount of whole mud can
ing will allow the boric acid solution be used.
to be sucked from the flask. After the 4. The temperature setting for distilling
25 ml is collected, remove stopper, the solution should be adjusted so it
and drain any liquid into the collec- does not cause boil-over (which
tion flask. Titrate the collection flask invalidates the test). It should boil
contents back to the original red/ the solution gently causing water (or
pink color with the 0.02 N H2SO4 distillate) to condense at the top of
solution and record the amount of the glass tubing. That way, the mud
acid used. is not boiled over into the receiving
8. The concentration of POLY-PLUST can flask but distillate merely collects in
be determined from the correct the tubing and runs down to the
graph. Remember to double the boric acid solution. Again, the tem-
result if a 5-ml sample is used. perature setting should be high
Additional guidelines and enough so a steady boil is main-
trouble-shooting tained, preventing the mud flask
1. It is important that the glass tubing from cooling and sucking boric acid
be flush with the bottom of the rub- into this flask.
ber stopper. If the glass tube protrudes
POLY-PLUST concentration (lb/bbl) 2.50
below the stopper, the caustic solu-
tion being distilled will collect around 2.00
the exposed tube and be sucked up 1.50
and over to the boric acid solution.
1.00
This will give high erroneous values
in the determination. 0.50
2. Be sure the indicator used is methyl 0.00
red. This indicator will change from 0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
a pale amber yellow to a pink or 0.02 N sulfuric acid
pinkish-red when going from high Figure 16: POLY-PLUS T (liquid) concentration test.
pH to low pH. Also, the boric acid
solution should turn the indicator
POLY-PLUST concentration (lb/bbl)
3.0
pink, not yellow. If it doesn’t turn 2.5
pink, obtain a fresh sample of boric 2.0
acid. If this is not possible, use 0.02
1.5
N sulfuric acid and add dropwise
1.0
until the solution just turns pink.
0.5
Use this solution to collect the dis-
tillate. This step will ensure that in 0.0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14
the final titration, only the acid 0.02 N sulfuric acid
required to titrate the ammonia will
be measured. Any addition of acid Figure 17: POLY-PLUS T (dry) concentration test.
to correct the boric acid is ignored.

CHAPTER
3 Testing
5. Be sure that the end of the glass 6. When the final titration is per-
tubing is below the surface of the formed, be sure to titrate back to
boric acid solution. It is even better the original color of the boric acid
if a Pasteur pipette is used at this solution. If a light pink was noted,
end instead of a glass tube. The do not continue to titrate to a
opening is smaller therefore the darker pink or reddish color.
chance of allowing ammonia to
escape is reduced.
Section 8. Chemical Analysis Relating to Corrosion
A) ZINC OXIDE (ZnO) AND BASIC ZINC 14. Add 10 ml glacial acetic acid
CARBONATE (ZnCO3•Zn(OH)2) (CAREFUL: Use a vent hood,
Purpose if available).
Zinc oxide and zinc carbonate may be 15. Stir 10 min with mixer or stirrer. If
used to scavenge hydrogen sulfide in neither is available, hand mix with
drilling fluids. In order to determine stirring rod. Thorough mixing is
the available ZnO or ZnCO3 in the essential as the reaction is slow to
mud, the following may be used: take place.
16. Add 15 ml ammonium hydroxide
Equipment
(CAREFUL).
11. Acetic acid, glacial.
17. Check pH. If pH is above 9, proceed
12. Ammonium fluoride, 10%.
to next step. If pH is below 9, add
13. Ammonium hydroxide,
additional ammonium hydroxide
concentrated.
in 5-ml increments until pH is
14. Masking Agent.
above 9, then proceed.
16. Deionized water.
18. Add 3 ml of Masking Agent.
17. Formaldehyde solution (4%).
19. Add 10 ml of ammonium fluoride
18. Calmagite Indicator solution.
solution.
19. Standard Versenate solution.
NOTE: Ammonium fluoride is poiso-
10. Beaker, 150-ml.
nous; do not pipette with your mouth.
11. Graduated cylinders: one 10-ml,
Never mix ammonium fluoride with
one 25-ml and one 100-ml.
an acidic solution.
12. Field mixer with powerstat or
10. Transfer the solution to the
magnetic stirrer with stirring bar.
100-ml graduated cylinder and
13. Syringes: one 10-ml and one 20-ml.
dilute to the 100-ml mark with
14. Plastic funnel, 4 in.
deionized water.
15. Fluted filter paper (S & S No. 588
11. Mix well and filter into a dry,
size 18.5 cm).
clean beaker.
16. pH strips.
12. Take 20 ml of filtrate and place in
17. Volumetric pipettes: one 10-ml
a clean beaker.
and one 20-ml.
13. Dilute with deionized water to
Procedure about 40 ml.
11. Stir the mud sample, then measure 14. Add 6 drops of Calmagite
10 ml using syringe. Indicator. If solution is blue,
12. Place in 150-ml beaker. proceed directly to Step 15. If
13. Dilute to 40 ml with deionized solution is red, titrate slowly with
water. Standard Versenate to the regular

CHAPTER
3 Testing
blue endpoint. The amount of CAUTION: This test should be used

Versenate indicator does not need only on steel equipment; do not use on
to be recorded. aluminum or metal plating because
15. Add 5 ml ammonium hydroxide. poisonous fumes may be formed.
16. Check the pH. It should be between NOTE: Information taken from
10 and 11. If pH is below 10, add “Corrosion of Oil and Gas Well
additional ammonium hydroxide Equipment,” Sponsored by National
in 5-ml increments until pH of 10 Association of Corrosion Engineers
is reached. International and American Petroleum
17. Add 5 ml formaldehyde solution. Institute, 300 Corrigan Tower Building,
18. Let stand at least 2 min. Solution Dallas, TX, 1958, page 85.
will turn from blue to wine-red if
C) HYDROGEN SULFIDE (H2S)
zinc is present.
19. Titrate with Versenate indicator Purpose
until wine-red changes to blue. It is possible for the poison gas, H2S to
Calculations enter the drilling fluid causing corro-
ZnO (lb/bbl) = sion. The gas is deadly poison to living
28.5 x ml of Standard Versenate beings. Two different methods are pre-
ml of sample x ml of filtrate sented for determination of H2S in parts
per million. The first method is rapid,
ZnCO3 (lb/bbl) = and requires a minimum of equipment.
44 x ml of Standard Versenate The results are less accurate, and should
ml of sample x ml of filtrate be used to indicate H2S as present or
not. Use the second method (GGT) to
B) IRON SULFIDE SCALE (QUALITATIVE)
determine ppm of H2S in the drilling
Purpose fluid by the use of the filtrate analysis.
To test for iron sulfide on steel equip-
ment, a special reagent solution is 1) PROCEDURE I: HACH TEST
used. While the presence of iron sul- Equipment

fide frequently indicates the presence 1. A special calibrated test bottle with
of H2S downhole, it by no means cap containing hole to release gas.
proves the existence of H2S gas. 2. Hydrogen sulfide test paper to fit
Equipment in cap.
Iron sulfide test solution, containing 3. Hypodermic syringe, one 10-ml.
15% HCl, 1% sodium arsenite and 4. Deionized water.
0.05% detergent used as a wetting agent. 5. Alka-SeltzerT tablets (fresh).
6. Color comparison chart for ppm H2S.
Procedure
7. Octanol defoamer.
A few drops of the acid solution is 8. Hydrochloric acid, approximately
placed on the equipment or scale being 6 N.
formed. If a bright yellow precipitate of
Procedure
arsenic sulfide is formed, the sample
1. With a syringe transfer 8.3 ml mud
contains iron sulfide. The precipitate
to test bottle. Add 16.7 ml deionized
looks like miniature “scrambled eggs.”
water and swirl until mixed. Volume
Since some iron will be dissolved by
is 25 ml now. To reduce foaming, a
the acid, a yellow-orange solution may
drop of defoamer should be added
result. This should not be mistaken for
at this point. Do not let the fluid
the yellow precipitate formed by the
touch and stain the paper.
sulfide. If bubbles are released, then
2. Place a circle of H2S test paper
the scale may have been carbonate
inside the test bottle cap (that has
from carbon dioxide, possibly.
CHAPTER
3 Testing
a hole in it for gas to escape contain air or oxygen, nitrogen is

through the paper). permitted).
3. Add an Alka-Seltzer tablet to the Section 4. Lead acetate paper disks
sample and immediately screw the (optional).
cap containing the test paper on Section 5. Sulfuric acid, approximately
the bottle. Gently swirl to stir. 5 N, reagent grade.
4. After 15 min, remove the test paper Section 6. Octanol defoamer.
and compare to the color chart. The Section 7. Hypodermic syringes: one
ppm H2S obtained from chart is mul- 10-ml with 21-gauge needle for acid,
tiplied by three to obtain the ppm one 40-ml and one 5-ml.
H2S in the mud. Procedure
This test will detect as little as 0.3 ppm 11. The gas train must be clean, dry
H2S. The test is only good for dissolved and on a level surface, since the
sulfide in mud. To determine an insolu- passages must be clear and mois-
ble sulfide, such as iron sulfide, it must ture may cause the flow meter ball
be put into solution with acid. Five to float erratically.
drops of hydrochloric acid at Step 3 12. Install a new CO2 cartridge.
will enable any iron sulfides to be 13. Add 20 ml deionized water to
determined. Chamber 1.
NOTE: If the H2S of mud is greater than 14. Add 5 drops of defoamer to
15 ppm, more dilution will be necessary. For Chamber 1.
concentrations between 15 and 125 ppm, 15. Select the correct sample volume
use 1 ml mud and 24 ml deionized water and Dräger tube for the expected
and multiply ppm H2S obtained from chart sulfide range from the following
by 25. table. Break the tip from each end
For concentrations between 125 and of the tube.
1,250 ppm, mix 1 ml mud in 9 ml 16. Install the tube with the arrow
deionized water in a small beaker, and pointed downward in the recepta-
take 1 ml of mix and add 24 ml deion- cle bored in the corner of the train.
ized water for the test; multiply ppm Also, install the clean, dry flow meter
H2S obtained from chart by 250. Since tube with the word “TOP” upward,
filtrate is used in GGT, these results will and the ball in the bored receptacle
not compare. in the side of the train. Be sure that
the O-rings seal around both tubes
2) PROCEDURE II: GARRETT GAS TRAIN
after they have been inserted.
Purpose 17. Measure out the filtrate sample
The Garrett Gas Train purges the H2S into Chamber 1. Chambers 2
from the filtrate prior to capturing the and 3 remain empty and serve
gas in a Dräger tube. as foam traps.
Equipment 18. Place O-rings on the chamber
Section 1. Garrett Gas Train and grooves and install the top of the
accessories. gas train. Hand tighten all screws
Section 2. Dräger H2S analysis tubes: evenly to seal the train.
A) Low range-H2S 100/a (100 to 19. Attach the flexible tubing to the
2,000 labeled) Factor = 0.12. dispersion tube and the Dräger
B) High range H2S 0.2%/A (labeled tube. The tubing does not need to
0.2 to 7%) Factor = 1,500. be clamped to the tubes and will
Section 3. CO2 cartridges (or other gas provide pressure relief in the event
which is inert to H2S and does not of over-pressurization.

CHAPTER
3 Testing
Sample Volumes and Tube Factor to be Used for Various Sulfide Ranges
Sulfide Range Sample Volume Dräger Tube Identification
(mg/l) (cm3) (see tube body) Tube Factor
1.2 - 24 10.0 H2S 100/a 0.12*
(100 - 2,000 range)
2.4 - 48 5.0 H2S 100/a 0.12*
(100 - 2,000 range)
4.8 - 96 2.5 H2S 100/a 0.12*
(100 - 2,000 range)
30 - 1,050 10.0 H2S 0.2%/A 1,500**
60 - 2,100 5.0 H2S 0.2%/A 1,500**

120 - 4,200 2.5 H2S 0.2%/A 1,500**
*Tube factor 0.12 applies to new tubes, H2S 100/a (Cat. No. CH-291-01), with scale 100 to 2,000. Old tubes use tube factor 12.0 with scale 1 or 2 to 20.
**Tube factor 1,500 applies to new tubes, H2S 0.2%/A (Cat. No. CH-281-01), with scale 0.2 to 7.0%. Old tubes with 1 to 17 cm scale use tube factor
600 times ratio: “batch factor”/0.40.
Table 6: Dräger tube identification and selected ranges.
10. Adjust the dispersion tube to the train. Take out the flow meter
approximately 0.5 cm above and Dräger tube and plug the holes
the bottom. with stoppers to keep dry. Wash
11. Gently flow CO2 for 15 sec to out the chambers with mild deter-
purge air from the system, then gent and a soft brush. Use a pipe
stop flow. Be sure to start the gas cleaner to clean out the passages
flow slowly so as not to blow the between chambers. Rinse the unit
ball out of the flow meter tube. with deionized water and allow to
You may also want to lightly cover drain dry.
the tube with a finger to make Calculations
sure the ball is not lost. Using the sample volume, the Dräger
12. Slowly inject 10 ml of sulfuric acid tube’s maximum darkened length and
into Chamber 1 through the rub- the factors, calculate the sulfides in
ber septum using the hypodermic the sample:
syringe and needle.
Sulfides (mg/l) =
13. Immediately restart CO2 flow.
darkened length x tube factor
Adjust the rate so the ball in the
ml of sample volume
flow meter tube is between the red
lines (200 to 400 cm3/min). One D) PHOSPHATE
CO2 cartridge should provide 15 Purpose
to 20 min of flow at this rate. The active ingredient in the inhibitors
14. Continue flowing for a total of CONQORT 404 and SI-1000E is an organic
15 min. Record the maximum phosphate. However, inorganic phos-
darkened length before any pre- phates may also be present in the
ceding “front” starts to smear. drilling fluid, thus the test must
Using high-range tubes, and sul- differentiate between organic and
fites in the filtrate, an orange inorganic phosphates.
color may be seen. The orange The following two procedures are
region should be ignored when basically the same, but using different
recording the darkened length. HACH kits.
15. The gas train MUST be cleaned to NOTE: Starch in the fluid may
avoid permanent damage caused prevent the detection of either organic
by the acid used. To clean, remove or inorganic phosphates.
the flexible tubing and the top of

CHAPTER
3 Testing
1) PROCEDURE I: USING HACH DIRECT reading of 0 mg/l or 100% trans-

READING COLORIMETER mittance depending on which
Equipment scale is being used.
11. Deionized water. 13. Place the prepared sample in the
12. Phenolphthalein indicator. colorimeter and read mg/l PO43–
13. PhosVer III pillows. or transmittance. If the mg/l PO43–
14. Potassium persulfate pillows. reading is greater than 2.0 or if the
15. Sodium hydroxide, 8 N NaOH. transmittance reading is less than
16. Sulfuric acid, 5 N H2SO4. 10%, repeat the procedure using
17. Erlenmeyer flask, 50-ml. less filtrate in Step 1.
18. Graduated cylinder, 25-ml. 14. Record mg/l PO43– reading for use
19. HACH Direct Reading colorimeter. in calculations. If the transmittance
10. Hot plate. scale is used, refer to the graph of
11. Pipettes: one 1-ml, one 5-ml and transmittance vs. mg/l PO43–.
one 10-ml. b) Total phosphate (inorganic
a) Inorganic phosphate plus organic)
11. Pipette 5 to 10 ml filtrate into the 1. Pipette 5 to 10 ml filtrate into the
50-ml flask. Add deionized water to 50-ml flask. Add deionized water to
the 20-ml mark. the 20-ml mark.
12. Add 1 ml sulfuric acid. 2. Add 1 ml sulfuric acid.
13. Boil for 15 min maintaining the 3. Add the contents of one potassium
volume at about 20 ml. persulfate pillow.
14. Cool. 4. Boil for 30 min.
15. Add one drop phenolphthalein 5. Boil down to not less than 10 ml
indicator. volume. Add deionized water, if
16. Add sodium hydroxide dropwise necessary.
until sample almost changes to pink. 6. Proceed as in Steps 4 through
If too much is added and the pink 11 above.
persists, add sulfuric acid dropwise NOTE: If the filtrate color disappears
until the pink color just disappears. due to the potassium persulfate oxida-
17. Pour sample into a 25-ml graduated tion, do not use the colored filtrate for
cylinder and add deionized water the blank in Step 11. In this case, use
to the 25-ml mark. deionized water.
18. Pour into square mixing bottle. 7. Insert the blank in the colorimeter.
19. Add the contents of one PhosVer Adjust the light control for a meter
III pillow. Swirl and let stand for reading of 0 mg/l or 100% transmit-
1 to 2 min (not over 2 min). tance depending on which scale is
10. Insert phosphate meter scale or being used.
transmittance scale into the HACH 8. Place the prepared sample in the
Direct Reading colorimeter and colorimeter and read mg/l PO43– or
use the 2408 color filter. % transmittance. If the mg/l PO43–
11. Fill another square colorimeter reading is greater than 2.0 or if the
bottle with the untreated filtrate transmittance reading is less than
for the blank. Make certain it is 10%, repeat the procedure using
the same concentration as the less filtrate in Step 15.
sample. If 5 ml is used for the sam- 9. Record mg/l PO43– reading for use in
ple, use 5 ml of the filtrate diluted calculations. If the transmittance
to 25 ml for the blank. scale is used, refer to the graph of
12. Insert the blank in the colorimeter. transmittance vs. mg/l PO43–.
Adjust the light control for a meter

CHAPTER
3 Testing
Calculations 18. Pour sample into the color

Inorganic phosphate (mg/l) = viewing tube.
mg/l of PO43– from chart x 25 19. Insert this tube into the color
ml of filtrate comparator in the opening nearest
the middle.
Total phosphate (mg/l) =
10. Put a blank in the other tube. Make
mg/l of PO43– from chart x 25
sure it is the same concentration as
ml of filtrate the sample. If 5 ml is used for the
Organic phosphate = sample, use 5 ml of the filtrate
total phosphate – inorganic phosphate diluted to 20 ml for the blank.
11. Hold the comparator up to a light
2) PROCEDURE II: HACH PHOSPHATE
and view through the two open-
KIT (PO-24)
ings in the front. Rotate the color
Equipment disc until a match is obtained. If
11. Deionized water. the color is too dark, repeat the
12. Phenolphthalein indicator. procedure using less filtrate in
13. PhosVer III pillows. Step 1.
14. Potassium persulfate pillows. 12. Record reading for use in
15. Sodium hydroxide, 8 N NaOH. calculations.
16. Sulfuric acid, 5 N H2SO4.
b) Total phosphate (inorganic
17. Erlenmeyer flask, 50-ml.
plus organic)
18. Graduated cylinder, 25-ml.
13. Pipette 5 to 10 ml filtrate into
19. HACH phosphate kit PO-24.
flask and add deionized water to
10. Hot plate.
the 20-ml mark.
11. Pipettes: one 1-ml, one
14. Add 1 ml sulfuric acid.
5-ml and one 10-ml.
15. Add contents of one potassium
a) Inorganic phosphate persulfate pillow.
11. Pipette 5 to 10 ml filtrate into the 16. Boil for 30 min.
50-ml flask. Add deionized water to 17. Boil down to not less than 10 ml
the 20-ml mark. volume. Add deionized water if
12. Add 1 ml sulfuric acid. necessary.
13. Boil for 15 min maintaining the 18. Proceed as in Steps 4 through
volume at about 20 ml. 10 above.
14. Cool. NOTE: If the filtrate color disap-
15. Add one drop of phenolphthalein pears due to the potassium persulfate
indicator. Add sodium hydroxide oxidation, do not use the colored fil-
dropwise until sample almost trate for the blank in Step 10. In this
turns pink. If too much sodium case, use deionized water.
hydroxide is added and the pink 19. Hold the comparator up to a light
persists, add sulfuric acid dropwise and view through the two openings
until pink color just disappears. in the front. Repeat the procedure
16. Pour sample into square mixing using less filtrate in Step 13.
bottle and add water up to the 20. Record reading for use in
20-ml mark. calculations.
17. Add a PhosVer III pillow to the
sample. Swirl and let stand for
1 to 2 min.

CHAPTER
3 Testing
Calculations sulfite is being added, H2S should be sus-

Inorganic phosphate (mg/l) = pected. (With sulfide present, the Cl– ion
reading Step 12 x 2 test may show an increase as it will react
ml of filtrate Step 1 with the ion also.)
Standardization of sodium thiosul-
Total phosphate (mg/l) =
fate solution.
reading Step 20 x 2
Sodium thiosulfate does not have
ml of filtrate Step 13 a long shelf life. Every two weeks it
Organic phosphate = should be checked against the KI-KIO3
total phosphate – inorganic phosphate solution as follows. This is important
as a weaker sodium thiosulfate solu-
E) OXYGEN SCAVENGER: tion will give you lower sulfite con-
SO32– CONTENT
tent and a deterioration factor must
Purpose be used.
Oxygen scavengers that contain 1. Pipette 2 ml of the “iodine” solution
ammonium bisulfite or sodium sulfite into a 125-ml beaker.
are added to some drilling fluids to 2. Add 2 drops of hydrochloric acid.
reduce dissolved oxygen to a mini- 3. Dilute with 10 ml deionized water.
mum. To assure the complete removal 4. Titrate with the sodium thiosulfate
of dissolved oxygen, an excess of the until most of the yellow color
sulfite (SO32–) ion should be maintained disappears.
in the mud. 5. Add 5 drops of starch indicator.
Two procedures are listed below: one 6. Continue titrating until the blue
used for normal filtrates and the other color just disappears.
used for dark filtrates. Use Procedure I 7. Record total ml of thiosulfate solu-
first as it is more accurate. However, tion required to calculate deteriora-
if the color change cannot be seen tion factor.
use Procedure II. Do not dilute filtrate 8. Use this factor in the equation for
with deionized water as this may add determining mg/l SO32– on dark
dissolved oxygen. colored filtrates:
Procedure: Light filtrates ml of KI-KIO3 solution
Factor =
Equipment ml of sodium thisulfate
1. Deionized water.
1) PROCEDURE I: LIGHT FILTRATES
2. Hydrochloric acid, 6 N HCl.
3. Standard “iodine” solution 0.008 N The mud sample for this test should
(KI-KIO3). be collected above the shaker. Because
4. Standard sodium thiosulfate of the instability of sulfite, the filtrate
solution, 0.008 N. should be collected and the test per-
5. Starch indicator solution. formed immediately.
6. Test tube. 1. Pipette 5 ml of filtrate into test tube.
7. Flasks, two 125-ml. (If amount of filtrate is limited, a
8. Pipettes: one 1-ml and one 2-ml. 1-ml sample may be used.)
NOTE: If any sulfide is present, it will CAUTION: Do not dilute sample for
also be titrated in this test. Determine this test.
hydrogen sulfide by some other method and 2. Add 5 drops of starch indicator and
subtract mg/l H2S x 2.4 from the mg/l 2 drops of hydrochloric acid.
SO32– obtained. If the SO32– content of the 3. Titrate with “iodine” solution until
mud is apparently increasing when no a permanent blue color develops.

CHAPTER
3 Testing
Calculations 3. Pipette 1 ml or more of the filtrate

SO32– (mg/l) = to both flasks. Flask No. 1 will be
ml of iodine solution x 320 the blank. Use white sheet of paper
ml of filtrate for background to better see color
change.
2) PROCEDURE II: DARK FILTRATES 4. To Flask No. 2, only add 4 drops
Use procedure for light filtrates if possi- of hydrochloric acid and 5 drops
ble, as it is simpler and more accurate. of starch indicator solution. The
However, if the color change cannot be solution will turn to a dark
seen, do not dilute the sample; proceed blue-black color.
with the dark filtrate procedure. If the 5. Titrate with sodium thiosulfate
filtrate is not too dark, a sample larger dropwise until the blue-black color
than 1 ml may be used. disappears and the color matches
1. Pipette 2 ml of “iodine” solution the blank solution in Flask No. 1.
into each of two 125-ml flasks.
2. Add 20 ml deionized water to each
flask.
Calculations
(ml of iodine solution – (factor x ml of sodium thiosulfate)) x 320.2
SO32– (mg/l) =
ml of filtrate
Section 9. Resistivity
Resistivity of the mud, filtrate and fil- 3. Measure the resistance in ohm-
ter cake is sometimes needed in order meters if using the direct reading
to help evaluate the electric logs. meter. The value should be set to
Equipment ohms if a “not direct meter” is
1. Mud, filtrate and filter cake. being used.
2. Direct reading resistivity meter for 4. Note the temperature of the
drilling fluids. measurement.
3. Calibrated resistivity cell. 5. Clean the cell, rinse with deionized
4. Thermometer, 32 to 220°F water and dry.
Procedure Calculations
1. Fill the clean, dry resistivity cell 1. Report the mud resistivity Rm or fil-
with freshly stirred mud or filtrate. trate resistivity Rmf in ohm-meters
Try to ensure no air bubbles are to nearest 0.01 units.
entrained. Fill the cell to the 2. Report the sample temperature in °F.
correct volume according to the 3. If the reading is in ohms, convert to
manufacturer’s procedure. ohm-meters by:
2. Connect the cell to the meter. 3. Resistance (ohm-meter) =
R (ohms) x K (cell constant, m2/m)

CHAPTER
3 Testing
Section 10. Glycol Testing Procedure (Field procedure

to determine the glycol content of a drilling fluid)
A) REFRACTOMETER
Equipment
1. Refractometer for determining the
glycol volume percent range used in
the mud system. Several types of
refractometers can be used. A com-
monly used type is the Atago N10E.
The instrument measures glycol con-
tents in the 0 to10% range. If for Figure 18: Refractometer.
some reason a range outside of this is
desired, check with the manufactures 6. Record the BRIX reading and using
specifications for a different range. the glycol calibration curve, convert
2. 10-, 20- or 50-ml retort, oil-free steel the reading to glycol volume percent
wool, complete with glassware. in the mud.
7. Glycol percent whole mud = glycol
Reagents
percent from calibration curve x
Glycol used in the drilling fluid.
liquid fraction of the mud. Liquid
Distilled or deionized water.
fraction of the mud is Fw.
Graduated cylinders, storage bottles.
Procedure I B) DUAL-TEMPERATURE RETORT
1. Prepare a glycol in water calibration ANALYSIS FOR GLYCOL SYSTEMS
curve. This curve is made by adding Glycol as the primary inhibitor in the
various volumes percent of glycol in GLYDRILT system will deplete from the
deionized water (typically 1 to 6% system as it is adsorbed onto shales. It
by volume is used). Run each mix- is therefore important to measure and
ture through the retort and plot on a control the level of the glycol in the
linear graph paper the corresponding drilling mud. This test procedure can
BRIX reading vs. the original volume be used to measure the concentration
percent of glycol added. BRIX is the of all types of glycols. This is not an
name of the unit of refractometer API defined test, but uses the API
measurement for determination of retort procedure.
the glycol. Equipment
2. Run a retort on the drilling fluid. API standard retort test kit, a 50-ml is
3. Record the volume percent liquid. preferable for accuracy. It must be fitted
4. Shake up the liquid collected in the with a temperature control, which will
graduated cylinder from the retort. permit heating at 302°F (150°C) and
5. Place 2 to 4 drops of the liquid 950°F (510°C).
from the retort on the clean refrac-
Procedure II
tometer prism surface. Make sure
1. Place a known volume of mud into
the entire prism is covered with the
the lower cup of the retort cell. It is
liquid and close the cap. Look into
important that this sample contain
the refractometer window with the
as little entrained air as possible. Insert
prism pointed toward a bright light
fine, oil-free steel wool as required
source (see Figure 18).
into the upper part of the cell.

CHAPTER
3 Testing
Assemble the cell and seal the threads C) CHEMICAL DETERMINATION OF

with high-temperature grease (Never- GLYCOL USING CENTRIFUGE
Seez) or equivalent to reduce leakage Procedure
through the threads. 1. Collect 8 ml of filtrate and transfer
2. Set temperature controller to 302°F this to a graduated centrifuge tube.
(150°C). Heat the retort until all the 2. Add 3 g of NaCl salt to the tube
water has been collected (approxi- and shake it well until most
mately 90 min). Note this volume of the salt is dissolved.
as V1. 3. Centrifuge the tube for 3 min.
3. Re-adjust the temperature controller 4. The glycol will have separated out of
to 950°F (510°C), and continue to dis- the saturated NaCl solution and will
till over the remainder of the liquid have formed a layer on the top. The
phase. Note the final volume as V2. volume of this layer can be found
Volume % of glycol = from the graduations on the tube.
(V2 – V1) x 100 Note this volume (V).
Sample volume of mud Volume % glycol in filtrate =
NOTE: the presence of other liquids V x 100
with high boiling points, such as lubri- volume filtrate (ml)
cants or oil will interfere with the results Volume percent glycol in whole mud
of this test. = volume % glycol in filtrate x liquid
fraction of mud (Fw). Where liquid
fraction (Fw) equals %/100 from mud,
and is obtained from the retort.
Section 11. KLA-GARDT Concentration
QUANTITATIVE DETERMINATION Procedure

A procedure has been developed for Section 1. KLA-GARDT standard solutions:
approximating the concentration of Prepare standard KLA-GARDT solutions
excess KLA-GARD.T The test procedure for comparison testing. To prepare a
is based on the strong reaction of 1 lb/bbl (3 kg/m3) KLA-GARDT solution
KLA-GARDT and the chemical Reinecke add 1 gram KLA-GARDT to 350 ml of tap
salt with the formation of a white pre- water. Known concentrations, from
cipitate. Detailed procedures and the 1 lb/bbl (3 kg/m3) to the highest level
materials needed for conducting the used, should be prepared. For exam-
test are described below. ple, 1, 3, 5, 7 and 9 lb/bbl (3, 9, 14,
Equipment and materials needed 20 and 26 kg/m3) standard solutions
1. Reinecke salt. should be prepared for most appli-
2. Containers with caps. cations. These standard solutions
2. Sample of KLA-GARD.T should be labeled with the date they
3. Syringe (optional). were prepared; they will only last
4. Micro-filters (optional). approximately one month unless
5. Distilled water. a bactericide is used.

CHAPTER
3 Testing
Section 2. Reinecke salt indicator: To Section 5. Having prepared the indica-

prepare the indicator solution, dis- tor solution, conduct the KLA-GARDT
solve approximately 3% by weight of test as follows:
the Reinecke salt into distilled water A) In small vials (one for each of
(tap water can be utilized if distilled is the prepared KLA-GARDT standard
not available). Only small amounts of solutions), place 40 drops of dis-
the indicator solution should be pre- tilled water and 8 drops of salt
pared because the shelf life is only 7 indicator solution and shake well.
to 10 days at temperatures below 65°F To these vials, add 8 drops of the
(18°C). At temperatures above that, KLA-GARDT standard solutions (a
the shelf life of the indicator solution different standard to each vial)
decreases rapidly. For this reason, we and shake for 5 sec. Seal and
recommend the indicator solution be label the vials with the known
stored in a refrigerator and that new KLA-GARDT concentrations.
solutions be prepared often. To pre- B) In a small vial, place 40 drops
pare a small quantity of the indica- of distilled water and 8 drops of
tor solution, dissolve 0.75 g of the Reinecke salt indicator solution
Reinecke salt into 24.25 g of distilled and shake well. To this vial, add
water. Allow to dissolve for at least 8 drops of the mud system filtrate
4 hr before use, then thoroughly shake and shake for 5 sec. Seal and label
the solution before using it. It is nor- the vial.
mal for some insoluble material to Section 6. Allow the precipitates to set-
remain on the bottom of the con- tle for about 30 min. Compare the
tainer after standing. This can be height of the precipitate for the fil-
filtered out as explained below. trate (unknown) to the standards.
Section 3. When testing for the Re-check results after 1 hr.
KLA-GARDT concentration, a sample Section 7. By matching the height of
of drilling fluid filtrate and a clear the precipitate in the system filtrate
sample of the Reinecke salt solution to the height of the precipitate in
are required. one of the standards, the concentra-
Section 4. Prepare a clarified quantity of tion of KLA-GARDT can be estimated.
the Reinecke salt solution by drawing Section 8. If viscosity or other factors
about 5 ml into a syringe, then forc- in the filtrate interfere with the test,
ing the solution through a micro-fil- use 80 drops of water instead of 40
ter securely attached to the syringe. drops for both the filtrate and the
Collect the clear fluid in a small vial. standards and repeat the test.
If the above equipment is not avail-
able, the Reinecke salt solution can
still be used without filtering.

CHAPTER
3 Testing
Section 12. Permeability Plugging Test Procedure

Equipment to lightly cover the O-ring on the
11. Cylindrical cell, one fitted to end cap to allow for easier installa-
accept 1⁄4-inch thick porous disc. tion. Install the set screws, check for
12. Heating jacket. alignment marks, align properly and
13. Spacer ring. tighten snugly into the recesses of
14. Two end caps (one with screen for the cell cap. Use the hardened steel
hydraulic end). set screws and coat them with
15. Two stems: one with quick con- Never-Seez to facilitate their tighten-
nect for hydraulic hose, the other ing and removal. Use the T-wrench
with valve for top of cell. from the other end to push the
16. Hydraulic pump with quick connect floating cap down against the end
hose and coupling. cell cap to remove any trapped air.
17. Hydraulic fluid. 13. Install and tighten the inlet valve
18. Piston with O-rings to separate stem with the nipple of the quick-
hydraulic fluid from mud. connect on it. The valve stem can
19. T-bar wrench for piston positioning. be filled by attaching it to the
10. Reservoir receiver cell with hydraulic pump and slowly operate
bleed-off valve. the pump with the release valve
11. Back pressure regulator attachment. closed. When the stem is full, open
12. Two thermometers. the pump pressure relief valve and
13. Two safety locking pins. use the T-wrench from the other
Procedure end to push the floating cap down
11. Preheat the heating jacket to the against the end cell cap to remove
desired temperature. Open the cell any trapped air.
and check all O-rings and replace 14. Turn the cell upright and fill cell
any damaged O-rings. Apply a thin with 300 ml of drilling mud. This
coating of silicone grease on the will be the outlet end. Place an
two O-rings on the floating piston. O-ring into the recess in the top
Screw the floating piston onto the end of the cell. Install the hydraulic
T-bar wrench and install the piston hose and with the hand pump,
into the bottom of the cell, working pump the mud to just within the
it up and down to ensure that the edge of the recess and then place a
piston moves freely in the cell. disk on top of the O-ring then dis-
NOTE: the bottom of the cell is the connect hose. NOTE: The disks must
end with the shorter recess. Position be soaked for at least 5 to 10 min in
the piston so that it is near the bot- freshwater prior to use when testing a
tom edge of the cell and unscrew it water-base mud. If an oil or synthetic
from the wrench. This will be the mud is being tested, then the disks
inlet end or may also be called the must be soaked 5 to 10 min in the
hydraulic end. representative base oil prior to use.
12. Before unscrewing the T-bar Disks must never be re-used.
wrench, position the piston flush 15. Install the end cap on the outlet
with the edge of the recess. Place an end. Use a silicone grease to lightly
O-ring in the recess of the inlet end cover the O-ring on the end cap
of the cell. Install the hydraulic cell to allow for easier installation. Be
end cap (bottom cap) into the inlet sure that the set screw recesses are
end of the cell. Use a silicone grease aligned with the set screws and

CHAPTER
3 Testing
then tighten the set screws snugly and/or filtrate will be near the tem-
against the cap. Next, install the perature at which the test is run and
outlet valve stem with a safety slowly opening the reservoir drain
valve into the end of the cell cap valve will minimize any splattering of
and close the valve. Then holding the fluid and potential contact with
the valve assembly, place the cell eyes, fingers and hands.
into the heating jacket until it bot- 18. Once the desired hydraulic pressure
toms out. Rotate the cell clockwise is applied, apply some pressure to
until the cell locks in place over the back pressure receiver not to
the alignment pin that is in the exceed 50 psi and slowly open the
bottom of the heating jacket. safety valve. After 30 sec, slowly
16. Install a metal thermometer in the open the drain valve on the reser-
thermometer well in the top of the voir and collect the mud and/or fil-
cell. Place the filtrate reservoir onto trate that comes out into a small
the top of the valve stem assembly glass beaker and continue to collect
ensuring that the small valve O-ring the fluid until the reservoir just
is in good condition and lock the blows dry. This should be recorded
reservoir in place by installing the as the spurt loss.
safety retaining pin. Next install 19. Close the drain valve on the receiver
the back pressure receiver device reservoir and maintain the desired
onto the top of the valve stem and pressure on the cell with the
lock into place with the safety hydraulic pump. The pressure will
retaining pin. Connect the quick decrease during the filtration of the
connect from the hydraulic pump mud so additional pressure will be
to the valve stem on the inlet end applied to the cell in order to main-
of the cell before applying pressure. tain a constant pressure. Maintain
Apply 200 psi on the cell and leave the pressure on the cell for 30 min
the valve on the pump closed. As occasionally bleeding of the liquid
the cell is heating up, there will collected in the reservoir. After
be an increase in pressure in the 30 min are completed, record the
cell due to the heating up of the total amount of liquid recovered
hydraulic oil in the cell. Maintain (excluding the spurt loss). Close the
the 200 psi pressure by releasing drain valve and open the pressure
the built-up pressure by opening release valve on the pump. While
the valve on the hydraulic pump. the back pressure is still applied,
17. Heat the cell to the desired tem- opening the pressure release valve
perature. The test temperature for on the pump will push the floating
this series of tests will be 150°F. piston to the bottom of the cell and
Record the time it takes to heat up allow for recovering of the hydraulic
to the desired temperature. Close oil back into the pump. Turn off the
the pressure release valve on the power to the heating jacket.
pump and apply the desired pres- 10. After the oil has been recovered in
sure to the cell with the hydraulic the pump, close the safety valve.
pump. Apply 1,500 psi working Remove the hydraulic quick con-
hydraulic pressure to the cell with nect from the cell. Close the back
the hydraulic pump. pressure source valve and then
NOTE: When working with the bleed off the back pressure from
heated, pressurized cell, ensure that all the receiver. After the pressure has
are wearing safety glasses. The mud been completely removed from

CHAPTER
3 Testing
the reservoir, remove the safety 12. Recover the disk and filter cake
retaining pin and remove the back and wash off same very lightly
pressure device from the reservoir. with freshwater or base oil if an
11. Either allow the cell to cool while oil mud is tested and measure
still in the heating jacket or carefully the filter-cake thickness in 32nd
remove the cell from the heating of an inch. The total fluid loss is
jacket and allow to cool by allowing calculated as follows:
to come to room temperature or Total fluid loss (ml) = spurt loss (ml) +
place the cell in the sink and cool 2 x (30 min fluid recovery (ml))
off with water. After the cell has
completely cooled off, hold the cell
such that the safety valve stem is
not pointing toward yourself or oth-
ers. Slowly open the safety valve to
remove any trapped pressure in the
cell. Repeat this process several times
to ensure that all pressure has been
released. Remove the top cell cap
of the cell and then turn the cell
upside down in the sink. Remove
the hydraulic end cap (bottom cell
cap) to expose the floating piston.
Screw the T-bar wrench into the pis-
ton and push down to force out the
mud and the disk out the opposite
end of the cell.
NOTE: This should be done care-
fully as too much applied pressure
will cause the mud to splatter out.
Completely disassemble the cell and Figure 19: Permeability plugging apparatus.
clean and dry the entire apparatus.
Section 13. Brookfield Viscometer

Used to Obtain Low-Shear-Rate Viscosity (LSRV)
The following standardized procedures cylindrical spindles (#1 through 4). The
are recommended when measuring LVDV-II+ is the most widely used vis-
LSRV of a FLO-PROT fluid. These proce- cometer. The LVDV-III model has a
dures are designed to allow accurate wider speed selection and also has a pro-
measurement of the unique viscosity grammable feature neither of which is
profile provided by a FLO-PROT fluid. necessary for FLO-PROT applications. The
Every effort should be made to use spindle viscosity ranges at 0.3 RPM using
these procedures in order to make the LVDV-II+ or LVDV-III are: #1 to
valid comparisons between wells. 20,000 cP, #2 to 100,000 cP, #3 to
Equipment 400,000 cP and #4 to 2,000,000 cP.
Testing will be made using the When ordering a Brookfield viscome-
Brookfield LVDV-II+ or LVDV-III ter specify LVDV-II+ or LVDV-III with
digital viscometer with guard leg and cylindrical spindles #1 through 4. The

CHAPTER
3 Testing
LV prefix designates the proper spring The fluid sample should be tested at the
torque for the viscosity ranges M-I same temperature as the other rheologi-
desires. Also Input voltage and fre- cal properties. Stir the sample while
quency should be indicated when heating to equalize the temperature
ordering. The units are available in throughout the sample. A Hamilton
115, 220 or 230 volts AC and 50 or Beach-type mixer with a rheostat may
60 cycle frequency. be used. Stir at a slow rate to avoid over-
Other necessary equipment includes shearing the fluid which may result in
the large heating cup (3.25 in. diame- polymer degradation. Avoid entrapping
ter by 4 in. deep) and a mixing device air while stirring. Entrapped air will
to heat the fluid sample evenly. result in erroneous readings.
Location Initializing the Viscometer
Locate the Brookfield where a stable While heating the sample, remove the
power supply is available. It should be rubber band holding the viscometer
located where vibrations from the rig are shaft in place. The viscometer uses a
minimal. Rig vibrations may contribute gem bearing and calibrated spring.
to inaccurately low LSRV measurements. Avoid impact and twisting of the shaft.
Dust may damage the electronics or the Always replace the rubber band when
bearings so a dust-free atmosphere not using the viscometer.
should be located. Turn on the viscometer. The digital
Setup screen will display the operations as
Remove the viscometer from the case. the viscometer autozeroes itself. The
Install gear assembly on stand with following screen descriptions are for
rack and insert Brookfield viscometer the LVDV-II+ viscometer, the most
post in assembly and tighten clamp widely used model.
screw. Level viscometer by rotating it When the power is on the screen will
slightly on the stand and/or by adjust- flash “Brookfield DV-II+ LV Viscometer,”
ing feet. Use the bubble level on the then “Version 3.0.” The screen then
top as a guide. automatically changes to “Remove spin-
Plug the temperature probe into the dle Press any key.” Press any of the yel-
receptacle on the back of the viscome- low keys and the display changes to
ter. Make sure the power switch on the “Autozeroing Viscometer.” After autoze-
rear of the viscometer is OFF. Plug the roing the screen will display “Replace
power cord into the receptacle on the spindle press any key.” Select the appro-
back of the viscometer and plug into priate cylindrical spindle for the desired
appropriate AC socket. “The AC input viscosity. Most applications will use
voltage and frequency must be within the the Number 2 spindle. Note that the
appropriate as shown on the name plate spindles are marked on the neck.
of the Viscometer.” NOTE: The LVDV-II+ Attach the spindle by threading it
must be earth grounded to ensure against onto the shaft. These are left-handed
electronic failure! threads. Hold the shaft in one hand
This is a delicate electronic instrument. to prevent damage to the spring and
Care should be taken to avoid power surges bearing while tightening the spindle.
and frequency variations. Disconnect the After tightening the spindle, press one
viscometer when not in use. of the yellow buttons on the key pad.
Pour the FLO-PROT fluid to be tested to The default display will appear on
within a 1⁄2 in. of the top of the heating the screen.
cup and heat to desired temperature.

CHAPTER
3 Testing
Viscometer display RPM. M-I is doing all testing at 0.3 RPM.

The screen will look something like this: When the proper value appears, press
the set speed key. NOTE: The vis-
% 0. 0 S 62 cometer is now running, press the
MOTOR ON/OFF key to stop the vis-
0.0 RPM 70.5°F cometer, but hold the desired speed
Values may vary according to what in memory. The value in the lower
was last tested. right is temperature as noted by the
The upper left corner displays vis- temperature probe.
cometer readings. These may be in The viscometer is now ready for
the following units: running a test.
% viscometer torque (%) NOTE: In order to have SI units dis-
cP viscosity (cP or mPa) played, hold the AUTO RANGE key
SR — Shear Rate (always 0 due to while turning on the viscometer. To get
spindle configuration) temperature in °C hold the Select Display
SS — Shear Stress (always 0 due to key while turning on the power.
spindle configuration) Testing
The default units for the LVDV-II+ is After setting up the viscometer and
%. The value in the upper left corner heating the sample to test temperature,
should be ~ +1.0% when not in use. A a test can be performed. Centralize the
value greater may indicate damage to heating cup beneath the viscometer.
the bearing or spring. Boundary effects caused by eccentric
M-I is using viscosity in cP (cen- placement may alter LSRV readings.
tipoise) as the standard reading. To Make sure the guard leg is in place to
select the appropriate units, press the avoid damage to the spindle, bear-
Select Display key until the cP value ings and spring. Lower the viscometer
appears. The SI unit mPa is equivalent until the recess in the spindle shaft is at
to cP (40,000 cP = 40,000 mPa). the top of the fluid. While lowering
The upper right-hand value is the the viscometer hold it under the front
spindle code. The code allows the vis- to prevent excessive vibration.
cometer to correctly calculate viscosity Set a timer for 3 min and turn on the
for a given spindle geometry. The code viscometer motor with the MOTOR
for the #2 spindle is S62 and for the ON/OFF button. Take viscosity readings
#3 spindle it is S63. If the correct code at 1, 2 and 3 min while the viscome-
is not on the screen, press “Select ter is running. These values should
Spindle” key. The S will blink. Use the be labeled LSRV1, LSRV2 and LSRV3,
orange up and down arrow keys to respectively. Part of the first min will
search for the correct spindle code. involve torquing the spring. Generally
When the correct code is found, press the fluid will reach its maximum vis-
the Select Spindle key and this code cosity within the three min time. The
will become the default code. 3-min reading may actually be less
This viscometer can test viscosity than the 2-min reading. If the 3-min
at 0.3, 0.5, 0.6, 1.0, 1.5, 2.0, 2.5, 3.0, reading is less than the 2-min reading
6.0, 10.0, 12.0, 20.0, 30.0, 50.0, 60.0 the spindle is probably slipping as it
and 100.0 RPM. To set the speed, “drills a holes in the fluid.”
press the orange arrow keys until the After the test, turn off the viscometer
desired speed appears to the right of and raise the spindle above the fluid.

CHAPTER
3 Testing
Clean up
Turn off the viscometer. Remove the
spindle, then the guard leg. Wash them
thoroughly. Replace the guard leg and
reinstall the rubber band on the shaft.
Keep the viscometer away from water
and dust and unplug it when not in
use to avoid power surges.
Calibration
Calibration fluids are available from
Brookfield and their agents. The vis-
cometer should be calibrated regularly.
The procedures are outlined in the
Brookfield Digital Viscometer
Operating Instructions Manual, which
is included with the viscometer. This
manual also contains more detailed
information not discussed here.
Address:
Brookfield Engineering
Laboratories, Inc. Figure 20: Brookfield viscometer and thermocup.
240 Cushing Street
Stoughton, MA 02072, USA
Tel: 617-344-4310
Fax: 617-344-7141
Section 14. Drill Pipe Corrosion Ring Coupons

Drill pipe Corrosion Ring Coupons made from steel identical to that of
that are placed in the drillstring is one the tool joint, to avoid galvanic corro-
technique for monitoring the drilling sion. This is usually impractical so a
fluid corrosion rate. The removal and steel similar to the drill pipe is used.
examination of rings after a period of Usually AISI 4130 is used with no dif-
approximately 100 hr exposure down- ficulty noted. If any steel other than
hole can be highly informative. The the 4130 is used, it should be noted
cause of corrosion, and type of corro- on the ring package/report form. The
sion may possibly be determined by rings are machined from cold drawn
this technique. seamless tubing, and usually are not
The examination of the scale, if any, quenched and tempered.
will indicate the dissolved gas that is There are plastic encapsulated
causing the damage. If the source is coupons that are available in limited
known, the type of chemical treatment areas for use in the drillstring. Each
may be more effectively selected for operation should compare the results,
better control. and experimentally determine the
The circular-ring-type corrosion proper correlation that would be
coupon, or “corrosion ring” as it is desired. Do not assume they are
called, should fit properly in the tool interchangeable in results.
joint box. Ideally, the ring should be
CHAPTER
3 Testing
The plastic encapsulated coupons completely. The information should

have a preweighed metal ring that is include the operator, well name,
heat sealed similar to a specimen in location and person with address/
metallography. The overall dimen- fax/phone number to contact with
sions of the coupon are similar to the results. The type of drilling fluid,
steel coupon to ensure a proper fit. location of rings in the string, type
Proper care in placement is necessary. of metallurgy if not AISI 4130, date
There can be a coating fracture then in and date pulled from the string is
the chips could plug the bit nozzles. also desired. The total hours run, and
To process the plastic encapsulated the depth in and depth out can be
ring, the plastic is broken away using a recorded. The chemical treatments
vise or other technique that will allow used could also be noted and copies
no damage to the metal band. The of the daily mud check enclosed.
scale, if any, is observed and tested. 3. Following the test period, remove the
The coupon then is cleaned just as a coupon ring, and wipe off all of the
steel coupon would be. The “K”-factor drilling fluid residue with a cloth.
calculations are different for each of The ring should be examined visually
the plastic encapsulated coupons. The for the severity of corrosion and for
calculation of the corrosion rate is per- any mechanical damage. If the ring
formed in the same manner as with looks “like-new,” then the rate is
the steel coupons. probably low. If severe corrosion is
evident, the cause of the corrosion
A) RING COUPON
should be determined promptly so
MONITORING PROCEDURE
remedial action can be performed
1. Drill pipe corrosion coupon rings
quickly. After the ring is dry, it is
should be kept in the drillstring for
suggested that it be replaced in the
a minimum of 40 hr. Exposures of
vapor inhibited paper, then in the
less than 40 hr should not be used
mailing envelope. The API RP 13B-1
because the initial corrosion rates are
supplement now states that oil or
unusually high and can give mis-
grease is NOT to be put on the
leading data. It is normal to run the
coupon before sending to the lab. For
coupons for approximately 100 hr.
many years they said to put oil on
The rings are run in pairs. The first
them. The oil or grease can interfere
in the Kelly Saver Sub, and the one
with the scale identification in the
downhole in the last joint of drill
laboratory, and is a nuisance to the
pipe above the collars. The rings are
lab when trying to clean the coupon.
left in the string for more than one
bit run if necessary. The total time B) LABORATORY COUPON ANALYSIS
in the string is recorded, not just 1. Before proceeding with a quantitative
rotating hours. evaluation of the corrosion rate of
Care should be taken to ensure that the ring, the ring should be rinsed
the recess space in the box joint is with a suitable solvent. This will
clean to prevent an interference with remove any oily residue that may
tool joint makeup, and mechanical have been added. Verify that the
damage to the ring. During the instal- coupon number agrees with the
lation, it has been suggested that a number on the shipping package. If
clean dry glove be used to place the it does not, proper communications
coupon ring in the tool joint. should be set up to resolve the dis-
2. The drill pipe corrosion ring form crepancy. If a number can not be
or envelope should be filled out seen clearly, or with the aid of a

CHAPTER
3 Testing
scope, note this. Do not report a Visual inspection

coupon ring number on the report if If corrosion is evident when the coupon
it can not be verified. Prior to clean- is removed from the string, it may be
ing and weighing, determine the due to either a pitting or a generalized
nature of the scale, if any. A magnet attack. The corrosion rates determined
will indicate an oxide, and possibly by the weight loss method assume a
oxygen corrosion. With the drop- generalized attack. Pitting rates from
wise addition of the Iron Sulfide Test the corrosion ring can not be made.
Solution, effervescence could indicate Mechanical damage to the ring can be
the presence of carbonates from the seen if the metal has cuts, dents or
dissolved acid gas, carbon dioxide. metal moved from the surface. In
The presence of iron sulfide is also some cases, the ring will exhibit a series
noted during this same test. A yellow of worn spots, indicating considerable
precipitate of arsenic sulfide would movement of the ring in the box recess
appear as “miniature scrambled area. Just being bent may not cause a
eggs” in nature. The mere presence high rate to be determined.
of a yellow color just may indicate Since the corrosion ring is exposed
some of the steel is dissolving from to the mud pumped down the drill
the coupon, and without the yel- pipe, the weight loss of the metal will
low/green precipitate, no sulfide include that removed by corrosion
should be noted on the report. and also erosion.
2. The ring should be cleaned with a Examination of the ring may reveal
detergent solution and a stiff bristle deep pitting with a relatively low weight
brush or equivalent. It may be nec- loss. This condition would indicate a
essary to dip the ring in inhibited more severe corrosion problem than if
15% hydrochloric acid one or more it were all generalized corrosion.
times to aid in removal of the cor- The pH and Pf should be at the
rosion products. The ring should be optimum for each water-base system.
scrubbed with detergent after each CONQORT 404 should be considered if
acid dip. When the ring is clean, the rate is higher than desired. Any
rinse with clear water and then bacteria problem should be addressed,
anhydrous acetone or methyl alco- and treated, as this can cause serious
hol to allow the ring to dry. (Always problems in the system also.
maintain proper safety precautions The normally accepted value for
when handling chemicals.) corrosion rates of freshwater muds
3. After the ring has been properly is 2 lb/ft2-y or less with no pitting
processed, then it should be noted. Values near the top of this
reweighed at least to the nearest range should be evaluated for the
milligram. The weight loss can be addition of proper chemical treat-
calculated. If there is significant loss ments and possible mechanical
of metal due to mechanical damage, alterations to the rig equipment.
it is recommended that Mechanical
Damage (MD) be noted, and all of the C) CALCULATION OF CORROSION RATES
calculations be shown at the bot- Corrosion ring coupons are available
tom of the ring report. The weight from drilling fluid service and supply
loss in g multiplied by the “K”- companies. The coupons are usually
factor, divided by the total hours supplied numbered, preweighed,
in the string yields the corrosion wrapped in a vapor inhibited wrapper
rate.

CHAPTER
3 Testing
along with a shipping envelope. The kg/m2-y =

coupon number is also recorded on wt loss (mg) x 10,000 x 365
the package along with a calculation 1,000,000 x area (cm2) x days exposed**
factor called “K”-factor. In the USA, wt loss (mg) x 87.60
most factors are offered to obtain the or =
*area (cm2) x hours exposed**
corrosion rate in lb/ft2-y. This value ** The total surface area of the ring is
may be changed into other units if used in these calculations.
desired with the aid of tables or other ** Time used based on total time in
equations. The difference in the weight the drillstring.
of the cleaned coupon before and after 2. Following are the conversion rates
the test period is determined by weigh- between the various units for steel
ing. This weight loss multiplied by the coupons:
“K”-factor divided by the total hours mpy = 24.62 x lb/ft2-y
will yield the corrosion rate. mpy = 5.03 x kg/m2-y
It is possible to have other laborato- lb/ft -y = 0.04 x mpy
2
ries recalculate corrosion rates by lb/ft2-y = 0.20 x kg/m2-y

reweighing the coupon at another kg/m2-y = 0.20 x mpy
facility. Always take extreme care in kg/m2-y = 4.90 x lb/ft2-y
weighing and recording the proper
data to ensure excellent integrity.
1. The corrosion rate in pounds per
square foot per year (lb/ft2-y) could
be calculated by the following for-
mula if a “K”-factor was not supplied:
lb/ft2-y =
wt loss (mg) x 144 x 365
453,600 x *area (in2.) x days exposed**
wt loss (mg) x 2,781
or =
*area (in2.) x hours exposed**

CHAPTER
3 Testing
Oil-Mud Testing (Including Diesel Oil,

Mineral Oil and Synthetic Fluids)
Section 1. Aniline Point Determination
This test determines the aniline point 4. Thermometer, 0 to 220°F.
of an oil. When diesel oil was popular 5. Heat source.
as an additive in muds, a high num- Procedure
ber near 150°F was preferred. A lower 1. Into the clean and dry test tube, add
number could indicate a potential for equal volumes of oil and aniline.
attack of the rubber/elastomer com- 2. Place the stopper with stirrer and
pounds in contact with the drilling thermometer into the neck of
fluid. Aniline is an aromatic organic the tube.
chemical, and oils similar in nature 3. While stirring, warm the mixture
would have a low (undesirable) until it changes from cloudy to a
aniline point. miscible/clear phase.
The oil and fresh (pure) aniline are 4. Remove the heat source, and con-
mixed in equal amounts, and temper- tinue until the mixture becomes trace
ature increased until they are miscible, cloudy. Read the thermometer at that
and clear in a tube. The temperature point, and record as the aniline point.
(°F) at which this happens, is the CAUTION: The aniline is a poison
aniline point. chemical, and extreme care is suggested
Equipment in handling it. Keep the chemical off
1. Aniline reagent, pure. body, hands, etc., and clothes. In case
2. Pyrex glass test tube. of serious contact, flush with water
3. Coiled wire through stopper about 15 min, while a physician
for stirring. is called for guidance.
Section 2. Density (Mud Weight)

Equipment bubble is mounted on the beam.
1. Density may be expressed as pounds Attachments for extending the
per gallon (lb/gal), pounds per cubic range of the balance may be used.
foot (lb/ft3), g per cubic centimeter 2. Thermometer.
(g/cm3), Specific Gravity (SG) or Procedure
pressure gradient. Any instrument 1. The instrument base should be set
of sufficient accuracy to permit up approximately level.
measurements within ±0.1 lb/gal 2. Measure and record the temperature
or ±0.5 lb/ft3 (±0.01 g/cm3) may of the mud. Fill the clean, dry cup
be used. The mud balance is the with mud to be tested; put on and
instrument generally used. The rotate the cap until firmly seated.
weight of a mud cup attached to Make sure some of the mud is
one end of the beam is balanced expelled through the hole in the
on the other end by a fixed coun- cap to free trapped air or gas.
terweight and a rider free to move 3. Wash with base oil or wipe the mud
along a graduated scale. A level from the outside of the cup.

CHAPTER
3 Testing
4. Place the beam on the support and Mud gradient in psi/ft =

balance it by moving the rider along lb/ft3 lb/gal g/cm3
or or
the graduated scale. The beam is bal- 144 19.25 2.31
anced when the bubble is on the Calibration
center line. The instrument should be calibrated
5. Read the density at the side of the frequently with freshwater. Freshwater
rider toward the knife edge. Make should give a reading of 8.33 lb/gal or
appropriate corrections when a 62.3 lb/ft3 (1.0 g/cm3) at 70°F (21°C).
range extender is used. If it does not, adjust the balancing
6. Report the density to the nearest screw or the amount of lead shot in
0.1 lb/gal or 0.5 lb/ft3 (0.01 g/cm3). the well at the end of the graduated
7. To convert to other units, use the arm as required.
following relationships:
Specific gravity or g/cm3 =
lb/ft3 lb/gal
or
62.3 8.345
Section 3. Viscosity and Gel Strength

Equipment to fill the receiving vessel to the
The following instruments are used 1-qt (946-ml) mark.
to measure the viscosity and/or gel 3. Report the result to the nearest
strength of drilling fluids: second as Marsh funnel viscosity.
1. Marsh funnel — a simple device for Report the temperature of the
routine measurement of viscosity. sample in °F or °C.
2. Direct-indicating viscometer — used B) ROTATIONAL VISCOMETER
for measurement of plastic viscosity,
Description
yield point and gel strength.
3. Thermometer. Direct-indicating viscometers are rota-
tional-type instruments powered by
A) MARSH FUNNEL means of an electric motor or a hand
Description crank. Mud is contained in the annu-
The Marsh funnel is dimensioned so lar space between two cylinders. The
that, by following standard procedures, outer cylinder or rotor sleeve is driven
the outflow time of 1 qt (946 cm3) of at a constant rotational velocity. The
freshwater at a temperature of 70±5°F rotation of the rotor sleeve in the mud
(21±3°C) is 26±0.5 sec. A graduated cup produces a torque on the inner cylin-
or 1-quart vessel is used as a receiver. der or bob. A torsion spring restrains
Procedure the movement. A dial attached to the
1. Cover the orifice with a finger and bob indicates displacement of the bob.
pour a freshly taken mud sample Instrument constants have been so
through the screen into the clean, adjusted that plastic viscosity and yield
dry, upright funnel until the liquid point are obtained by using readings
level reaches the bottom of the from rotor sleeve speeds of 600 and
screen (1,500 ml). 300 RPM. The apparent viscosity in
2. Quickly remove the finger and mea- centipoise equals the 600-RPM reading
sure the time required for the mud divided by 2.

CHAPTER
3 Testing
CAUTION: These Direct-Indicating 2) PROCEDURE: GEL STRENGTH

Viscometers are designed for a maximum 1. Place the mud sample in position
temperature of 200°F (93°C) in unpressur- as above. Stir at high speed for
ized fluids. If fluids above 200°F (93°C) 10 sec.
are to be tested, the operator should use 2. Allow the mud to stand undis-
a solid metal bob. Liquid trapped inside turbed for 10 sec with the motor
a hollow bob may vaporize and cause off. With the clutch in neutral,
the bob to explode when immersed in slowly and steadily turn the hand-
high-temperature fluid. wheel in a counterclockwise direc-
tion to produce a positive dial
1) PROCEDURE: PLASTIC VISCOSITY, YIELD
POINT AND APPARENT VISCOSITY
reading. The maximum reading is
the initial gel strength in lb/100 ft2.
1. Place a sample of mud in a ther-
For instruments having a 3-RPM
mal cup and immerse the rotor
speed, the maximum reading
sleeve exactly to the scribed line.
attained after starting rotation at
Measurements should be made
3 RPM is the initial gel strength.
with a minimum delay from the
Report the temperature of the
time of sampling. Tests should be
sample in °F or °C.
conducted at either 120±2°F
3. Restir the mud at high speed for
(50±1°C) or 150±2°F (65±1°C).
10 sec and then wait 10 min. Repeat
(Operators may require testing
the measurement as before and
at additional temperatures.)
report the maximum reading as the
2. Heat or cool the mud sample to the
10-min gel strength in lb/100 ft2.
selected temperature. The sample
Report the temperature of the
should be sheared at 300 RPM while
sample in °F or °C.
heating or cooling to ensure a uni-
4. In some instances, a 30-min gel
form sample temperature. Record
strength measurement may also
the temperature of the sample.
be required. To conduct the 30-min
3. With the sleeve rotating at 600 RPM,
gel strength, repeat the 10-min gel
wait for the dial reading to reach a
strength procedure as above but
steady value (the time required is
allow the fluid to stand undisturbed
dependent on the mud characteris-
for 30 min.
tics). Record the dial reading for
600 RPM. Calibration
4. Shift to 300 RPM and wait for the Operation of the instrument as a
dial reading to come to a steady direct-indicating viscometer depends
value. Record the dial reading for upon maintenance of the correct
300 RPM. spring tension and the correct speed
5. The Plastic Viscosity (PV) in cen- of sleeve rotation. Procedures are avail-
tipoise equals the 600-RPM reading able from the manufacturer to test
minus the 300-RPM reading. The spring tension and speed. Generally,
Yield Point (YP) in lb/100 ft2 equals however, a simpler test of reliability of
the 300-RPM reading minus the the instrument can be made by mea-
plastic viscosity. Report the tem- suring a Newtonian liquid of known
perature of the sample in °F or °C. viscosity (e.g. silicone liquids, sugar
The Apparent Viscosity (AV) in cen- solutions or petroleum oils of known
tipoise equals the 600-RPM reading viscosities at specified temperatures).
divided by 2.

CHAPTER
3 Testing
Section 4. Filtration
HIGH-TEMPERATURE, NOTE: Each filter or fiberglass backed

HIGH-PRESSURE TEST filter can be used only ONCE!
Equipment Due to the expansion of the fluid
CAUTION: Carefully observe the recom- while heating it is necessary to leave
mendations of the manufacturer on limi- space in the heating cell to prevent
tations on sample volume and pressure over pressurization.
for the temperature to be used. Recommended head gaps.
The instruments consist essentially Temperature Empty Space
of a controlled pressure source, a cell (°F) (in.)
designed to withstand a working pres- Up to 300 1
sure of at least 1,000 psi (70.3 kg/cm2), a 300 - 400 1.5 - 2
400 - 500 2.5 - 3
system for heating the cell, and a suit-
able frame to hold the cell and heating It is also necessary to apply pressure
system. For filtration tests at tempera- to the filtrate receiver to prevent boil-
tures above 200°F (93.4°C), a pressuring the filtrate. The recommended
ized collection cell should be designed back-pressures for various tempera-
to withstand a working back pressure of tures are as follows (the top pressure
at least 500 psi (35.3 kg/cm2) to avoid must be adjusted to maintain the
flashing or evaporation of the filtrate at proper differential):
high temperatures.
The filter cell is equipped with a ther- Temperature Bottom Pressure
(°F) (psi)
mocouple or thermometer, thermome- Up to 300 100
ter well, oil-resistant gaskets, and support 300 - 400 200
for the filter medium. For tempera- 400 - 500 300
tures to 350°F (177°C) use filter paper
(Whatman No. 50 or equivalent). For Procedure for temperatures not
temperatures above 350°F (177°C) use above 350°F (177°C)
a Dynalloy disc for each test. API cur- 1. Connect the heating jacket to the
rently does not have a recommended correct voltage for the unit before
procedure for temperatures above 400°F the test is to be made. Place a ther-
(204°C). A non-hazardous gas such as mometer in the thermometer well.
nitrogen (preferred) or carbon dioxide Preheat the heating jacket to 10°F
should be used for the pressure source. above selected test temperature.
Above 300°F (149°C), only nitrogen Adjust the thermostat in order to
should be used. WARNING: Do not use maintain the desired temperature.
N2O for this test, as the cartridges may 2. Stir the mud sample for 5 min.
allow the cell to explode. The API warns Prepare the cell with the mud sam-
against this usage. ple then filter paper, taking care
For stirring a sample, if possible not to fill the cell closer than 1 in.
use a high-speed mixer, 11,000 to (2.5 cm) from the top to allow
17,000 RPM under load, with single, for expansion.
corrugated impeller approximately 3. Place the cell into the heating jacket
1 in. (25 mm) in diameter (e.g. with both top and bottom valves
Multimixer or Hamilton Beach) and closed. Transfer the thermometer
a container such as Hamilton Beach to the cell thermometer well.
mixer cup No. M 110-D. 4. Place the pressure unit on the top
valve and lock in place. Lock the

CHAPTER
3 Testing
bottom pressure receiver to the top to allow for expansion, then place
bottom valve. Apply 200 psi the appropriate filtration medium.
(14.06 kg/cm2) to the top pressure 4. Place the cell into the heating jacket
unit and 100 psi (7.03 kg/cm2) to with both top and bottom valves
the bottom pressure unit while closed. Transfer the thermometer to
keeping the valves closed. Open the cell thermometer-well.
the top valve and apply 200 psi 5. Place the pressure unit on the top
(14.06 kg/cm2) to the mud while valve and lock in place. Lock the
heating to the selected temperature. bottom pressure receiver to the bot-
5. When the sample reaches the tom valve. For testing at tempera-
selected temperature, increase the tures from 300 to 400°F (149 to
pressure of the top pressure unit to 204°C) apply 300 psi (21.1 kg/cm2)
600 psi (42.18 kg/cm2) and open to both pressure units with the
the bottom valve to start filtration. valves closed. Open the top valve
Collect the filtrate for 30 min main- and apply 300 psi (21.1 kg/cm2) to
taining the elected temperature the mud while heating.
within ±5°F. If back pressure rises 6. When the temperature of the sample
above 100 psi (7.03 kg/cm2) during reaches the selected test temperature,
the test, cautiously reduce the pres- increase the pressure of the top pres-
sure by drawing off a portion of the sure unit to 800 psi (56.2 kg/cm2)
filtrate. Record the total volume. and open the bottom valve to start
6. The filtrate volume should be cor- filtration. Collect the filtrate for
rected to a filter area of 7.1 in.2 30 min, maintaining the test tem-
(45.8 cm2). If the filter area is 3.5 in.2 perature at ±5°F. Maintain the initial
(22.6 cm2), double the filtrate volume back pressure during the test; cau-
and report. tiously reduce the pressure by draw-
7. At the end of the test, close both ing off a portion of the filtrate. Allow
valves. Back the T-screw off and sufficient time for all filtrate to drain
bleed pressure from both regulators. from the receiver, and record the
CAUTION: Pressure in the filter cell total volume. Time of heating of the
will still be approximately 500 psi sample in the filter cell should not
(35 kg/cm2). Maintain cell in upright exceed one hour.
position and cool to room temperature CAUTION: Testing at high tempera-
before disassembling. tures and high pressures will call for
Procedure for temperatures between added safety precautions. Pressuring
300 to 400°F (149 to 204°C) systems and filtrate receivers should
1. Connect the heating jacket to the be equipped with suitable safety relief
correct voltage for the unit before valves. Heating jackets should be
the test is made. Place a thermome- equipped with both an overheat safety
ter in the thermometer well. Preheat fuse and thermostatic cutoff. Vapor
the heating jacket to 10°F above the pressure of the liquid phase of muds
selected test temperature. Adjust the becomes an increasingly critical design
thermostat to maintain the desired factor as test temperatures are raised.
temperature. CAUTION: Pressure in the filter cell
2. Stir the mud sample for 10 min. will still be approximately 500 psi
3. Prepare the cell with the stirred mud (35 kg/cm2). Maintain cell in upright
sample taking care not to fill the cell position and cool to room temperature,
closer than 11⁄2 in. (38 mm) from the bleed all pressure before disassembling.

CHAPTER
3 Testing
Section 5. Activity
The equation for the activity curve using calcium chloride salt is:
AW = 1.003 + [(4.66079 x 10 –3) x (% by wt CaCl2)] – [(7.2903 x 10 –4) x
(% by wt CaCl2)2] + [(5.6323 x 10 –6) x (% by wt CaCl2)3]
Section 6. Electrical Stability

1. An electrical stability meter is used
to measure the relative stability of a
water-in-oil emulsion. This measure-
ment is made using a pair of accu-
rately and permanently spaced
electrode plates which are immersed
in a fluid sample. A DC power source
is used to provide an AC voltage
which is applied to the electrode at
a constant rate of voltage increase.
The voltage at which the emulsion Figure 21: Electrical stability meter.
becomes conductive is indicated by reading. The older manual type
current flow between the electrode requires that the power source but-
plates, completing the circuit will (1) ton is depressed manually and held
illuminate the indicator bulb when during the entire test while a dial is
using a manual dial meter or (2) cause turned. Do NOT move the electrode
the numerical reading to stabilize during measurements.
when using a direct reading meter. 5. a) If using the newer style direct
2. Thermometer. reading electrical stability meter,
Procedure depress and hold down button
1. Place a sample which has been until displayed value stabilizes.
passed through a 12 mesh screen Record the displayed value as
(Marsh Funnel Screen) in a con- the electrical stability (volts).
tainer assuring that the fluid has b) If using the older style manual
been stirred well. dial electrical stability meter,
2. Heat or cool the sample to 120±5°F depress and hold down red but-
(50±2°C). Record the temperature at ton while starting from a zero
which the electrical stability reading reading, increase the voltage
was taken. by moving the dial in a clock-
3. After inspecting cleanliness of the wise direction at a rate of 100 to
electrode, immerse the electrode 200 volts per second. Continue
into the mud. Hand stir the sample increasing the voltage until the
with the electrode for approximately indicator light illuminates. When
10 sec. Hold the electrode motion- the indicator light illuminates,
less and do not allow the electrode the voltage ramp has ended.
to touch the sides or bottom of the Calculation for the older style man-
container when taking a reading. ual dial electrical stability meter:
4. There are two types of stability Electrical stability (volts) =
meters available. The newer, most dial reading x 2
recent meter uses an automatic direct
CHAPTER
3 Testing
6. Clean electrical probe and repeat test. 7. Record the average of the two meas-
The two readings should not differ urements as the electrical stability.
by more than 5%. If the readings dif-
fer by more than 5%, check meter
and electrical probe for malfunctions.
Section 7. Liquid and Solids

Equipment sample cup. Liquid steel wool is
1. A retort is used to determine the NOT approved by API.
quantity of liquids and solids in the 16. Fill the retort sample cup with
drilling fluid. Mud is placed in a steel gas-free oil mud.
container and heated until the liquid 17. Place the lid on the sample cup
components have been vaporized. and allow the mud overflow to
The vapors are passed through a con- pass through the hole in the lid.
denser and collected in a graduated To ensure a correct volume of
cylinder, and the volume of liquid is sample, some mud must flow
measured. Solids, both suspended through the hole.
and dissolved, are determined by dif- 18. Wipe the overflow from the
ference. A 10, 20 or 50 ml retort sample cup and lid.
may be used in determining the liq- 19. Place a clean, dry receiver under
uid and solids content. To reduce the condenser discharge.
the amount of error associated with 10. Heat the retort, continuing for
entrained air, a 20 or 50 ml retort 10 min beyond the time that no
is recommended. more condensate is being dis-
Procedure charged from the condenser.
11. Be sure the retort, condenser and 11. Remove the liquid receiver from
liquid receiver are clean, dry and the retort. Note the total volume
cooled from the previous use. of liquid recovered. If solids are
12. Collect a sample of mud and allow present in the liquid, whole mud
it to cool to approximately 75±2°F has boiled over and the procedure
(24±1.4°C) or ambient tempera- MUST be repeated.
ture. Screen the sample through 12. Record the volumes of oil and
a 12 mesh screen to remove lost- water in the liquid receiver after it
circulation material and large has cooled to 75±2.5°F (24±1.4°C)
cuttings. or ambient temperature.
13. If the mud contains gas or air, 13. From the volumes of oil and water
slowly stir 2 to 3 min to remove collected and the volume of the
the gas. original mud sample, calculate the
14. Lubricate the threads on the sample percent by volume oil, water and
cup and condenser tube with a light solids of the mud.
coating of Never-Seez (this is the 14. All solids — both suspended and in
only material to be used according solution — will be retained in the
to API procedures). This prevents retort. For muds containing sub-
vapor loss through the threads. stantial quantities of salt, calcula-
15. Lightly pack a ring of steel wool tions of suspended solids content
into the retort chamber above the will be in error unless corrections
are made for the dissolved salt.

CHAPTER
3 Testing
Section 8. Chemical Analysis of Oil-Base Drilling Muds
A) ALKALINITY (Pom) (VSA•API) disappears. Continue stirring and if

The alkalinity of an oil mud is deter- no pink color reappears within one
mined by breaking the emulsion and min, stop stirring. It may be neces-
titrating the mixture rapidly to the sary to stop stirring and allow the
first color change or endpoint. The mixture to separate into two phases
number of ml of 0.1 N sulfuric acid to more clearly see the color in the
used in the titration per ml of mud is aqueous phase.
reported as the alkalinity of the mud 6. Let the sample stand for 5 min. If
or POM. no pink color reappears, the end
Two testing procedures will be dis- point has been reached. If the pink
cussed which use different solvents. The color returns titrate a second time
first procedure is an effective test for oil- with sulfuric acid. If pink color
base fluid using either barite or hematite returns a third time titrate again.
in a single-salt system. The second pro- Do not titrate after the third time.
cedure is not as accurate but is required 7. Pom = ml of 0.1 N H2SO4
when using a two-salt system. per ml mud.
Equipment and reagents 8. Excess lime (lb/bbl) = Pom x 1.295.
1. Titrating assembly (magnetic stirrer B) SALINITY — CHLORIDES IN THE
or Hamilton Beach stirrer). WHOLE MUD
2. 5-ml pipette. Reagents
3. 16-oz Mason jar, 500-ml beaker • Potassium Chromate Indicator.
or equivalent. • 0.282N AgNO3 solution.
4. Xylene-isopropyl alcohol mixture The chloride titration is a continua-
(50:50) or Propyl Propasol. tion of the alkalinity measurement. To
5. Phenolphthalein Indicator. the sample that has just been checked
6. Sulfuric acid solution, 0.1N H2SO4. for alkalinity, add 10 to 15 drops of
Procedure potassium chromate indicator. Titrate
1. When using Testing Procedure #1, with 0.282N AgNO3 while stirring
put 100 ml of Xylene/IPA blend or until the first color change occurs.
75 ml of Propyl Propasol in glass jar. This is the endpoint. Do NOT titrate
Fill a 5-ml syringe with whole mud to “brick red.”
to past the 3-ml mark. API requires the salt content to be
2. Disperse 2 ml of oil mud into the expressed as total chlorides in the
solvent and add 200 ml of distilled mud phase calculated as below:
water. Total Cl– in mud (mg/l) = ml of 0.282
3. Add 15 drops of phenolphthalein. N AgNO3 x 10,000 per ml mud
4. Stir rapidly with a magnetic stirrer, The chloride content can also be
Hamilton Beach stirrer or equivalent. expressed in other units depending on
5. While stirring, slowly titrate with the operating company, the information
0.1N H2SO4 until the pink color just desired and the mud system.

CHAPTER
3 Testing
Two salt systems (CaCl2/NaCl) fast enough to agitate the aqueous

In two salt or binary salt systems, it is phase without remixing the upper
necessary to test the mud for the cal- and lower phases.
cium chloride concentration by the cal- 10. Titrate very slowly with 0.1 molar
cium titration procedure described EDTA or Strong Versenate solu-
below. This measurement is required tion. A very distinct color change
along with the previous titration for salt from the reddish color to a blue-
content to determine the amounts of green color indicates the end
NaCl and CaCl2 present in the system. point has been reached.
Equipment C) WHOLE MUD
1. Titrating assembly (magnetic stirrer CALCIUM CALCULATION
with stirring bar or Hamilton Beach 4,000(0.1m EDTA, cm3)
mixer stirrer). Camud =
2.0 cm3
2. 5-ml pipette.
Nomenclature
3. 6-oz Mason jar with cap.
Pom = Whole mud alkalinity
4. Xylene-isopropyl alcohol mixture
Camud = Whole mud calcium
(50:50) or Propyl Propasol.
Clmud = Whole mud chlorides
5. Calver II Indicator powder.
Vo = % by volume oil from retort
6. 8N sodium hydroxide buffer solution.
Vw = % by volume water from retort
7. 5-ml syringe.
8. Deionized water. Example
9. EDTA solution (Strong Versenate or Pom = 3.0 cc
equivalent) 0.1 molar, 1 ml = 4,000 Whole mud
mg/l calcium), also known as “x 10 calcium – Camud = 33,600 mg/l
strong.” Whole mud
chlorides – Clmud = 100,000 mg/l
Procedure
% Oil – Vo = 59.5%
11. Add 100 ml of 50/50 xylene/
% Water – Vw = 25.0%
isopropanol solvent or 75 ml of
Propyl Proposal to jar. Binary Salt (CaCl2/NaCl)
12. Fill 5-ml syringe with whole oil Calculations and Conversions
mud past the 3-ml mark. 11. Calculate lime content in lb/bbl.
13. Displace 2 ml of oil mud into Limelb/bbl = Pom x 1.295
the jar. Limelb/bbl = 3.0 x 1.295 = 3.89
14. Cap the jar tightly and shake for 12. Calculate CaClmud content where
1 min. CaClmud = mg CaCl2/l
15. Add 200 ml deionized water to of whole mud
the jar. CaClmud = 2.774 x Camud
16. Add 3 ml 1N sodium hydroxide CaClmud = 2.774 x 33,600
buffer solution. = 93,206 mg/l
17. Add 0.1 to 0.25 g Calver II 13. Calculate pounds per bbl of CaCl2
Indicator powder. CaCl2(lb/bbl) = 0.000971 x Camud
18. Recap the jar and shake again for CaCl2(lb/bbl) = 0.000971 x 33,600
2 min. Set jar aside for 15 to 30 sec = 32.6 lb/bbl
to allow the two phases to separate. 14. Calculate chloride ion associated
If a reddish color appears in the with CaCl2 where ClCaCl =
aqueous (lower) phase, this indicates mg Cl–/l of whole mud
that calcium is present. ClCaCl = 1.77 x Camud
19. Place jar on the magnetic stirrer or ClCaCl = 1.77 x 33,600 = 59,472 mg/l
Hamilton Beach mixer. Stir only

CHAPTER
3 Testing
15. If ClCaCl is larger than or equal to NaClmax = 26.432 – 1.0472(WgtCaCl)

Clmud, then assume that only CaCl2 + 7.98191 x 10–3(WgtCaCl)2 +
is present in the mud and the sys- 5.2238 x 10–5(WgtCaCl)3
tem is not a binary salt system. NaClmax = 26.432 – 1.0472 x 22.73 +
If ClCaCl is less than Clmud, then 7.98191 x 10–3 x 22.732 + 5.2238 x
assume that both CaCl2 and NaCl 10–5 x 22.733 = 7.37
(binary salt system) are present If the calculated maximum amount
in the mud system. Proceed with of soluble NaCl (NaClmax) from
calculations. calculation #11 is less than the
16. Calculate the chloride ion calculated % by wgt NaCl from
associated with NaCl where calculation #10, the aqueous
ClNaCl = mg Cl–/l of mud phase salinities calculated in cal-
from NaCl culations #9 and #10 are incor-
ClNaCl = Clmud – ClCaCl rect because all of the NaCl is
ClNaCl = 100,000 – 59,472 not actually in solution.
= 40,528 mg/l 12. A new NaClmud must be calculated
17. Calculate the NaCl content where using the following “Fraction”
NaClmud = mg NaCl/l of mud calculation.
NaClmud = 1.65 x ClNaCl NaClmax(Calculation #11)
NaClmud = 1.65 x 40,528 Fraction =
WgtNaCl(Calculation #10)
= 66,871 mg/l
Fraction = 7.37 / 16.31 = 0.4519
18. Calculate the pounds per bbl of NaCl
13. New NaClmud = Old NaClmud x
NaCllb/bbl = 0.00035(NaClmud)
Fraction
NaCllb/bbl = 0.00035 x 66,871
New NaClmud = 66,871 x .4519
= 23.4 lb/bbl
= 30,219 mg/l
Calculations for determining the 14. Redo calculations #9 and #10 sub-
aqueous phase salinity stituting the New NaClmud into
19. Calculate the % by weight the formulas.
CaCl2(WgtCaCl)
WgtCaCl =
% by wgt CaCl2 = WgtCaCl =
100 x 93,206
100(CaClmud)
93,206 + 30,219 + 10,000(25.0)
CaClmud + NaClmud + 10,000(Vw)
= 24.96% by weight
WgtCaCl =
100 x 93,206 WgtNaCl =
93,206 + 66,871 + 10,000(25.0) 100 x 30,219
93,206 + 30,219 + 10,000(25.0)
= 22.73% by weight
10. Calculate the % by weight = 8.09% by weight
NaCl(WgtNaCl) 15. With the new WgtCaCl and WgtNaCl,
% by wgt NaCl = WgtNaCl = calculate the new NaClmax
100(NaClmud) (Calculation #11)
CaClmud + NaClmud + 10,000(Vw) NaClmax = 26.432 – 1.0472 x 24.96 +
7.98191 x 10–3 x 24.962 + 5.2238 x
WgtNaCl =
10–5 x 24.963 = 6.08
100 x 66,871
16. Calculate the New Fraction
93,206 + 66,871 + 10,000(25.0)
(Calculation #12).
= 16.31% by weight
Fraction = 6.08 / 8.09 = 0.7515
11. Using the mutual solubility calcu-
lation for NaCl/CaCl2 brine solu-
tions, calculate the maximum
amount of soluble NaCl (NaClmax)

CHAPTER
3 Testing
17. Continue the calculations (#11 0.007923(WgtCaCl) +

through #16) until the “Fraction” 0.00008334(WgtNaCl)(WgtCaCl) +
is greater than 0.95. 0.00004395(WgtNaCl)2 +
New NaClmud = Old NaClmud x 0.00004964(WgtCaCl)2
Fraction BrineSG = 0.99707 + 0.006504(5.82)
New NaClmud = 30,219 x .7515 + 0.007923(25.58) +
= 22,710 mg/l 0.00008334(5.82)(25.58) +
WgtCaCl = 0.00004395(5.82)2 +
100 x 93,206 0.00004964(25.58)2
93,206 + 22,710 + 10,000(25.0) BrineSG = 1.28 g/cm3
21. Calculate the CaCl2 concentration
= 25.47% by weight
in mg/l
WgtNaCl = CaCl2, mg/l =
100 x 22,710 10,000(WgtCaCl)(BrineSG)
93,206 + 22,710 + 10,000(25.0) CaCl2, mg/l = 10,000(25.58)(1.28)
= 6.21% by weight = 327,424 mg/l
NaClmax = 26.432 – 1.0472 x 25.47 + 22. Calculate the NaCl concentration
7.98191 x 10–3 x 25.472 + 5.2238 x in mg/l
10–5 x 25.473 = 5.80 NaCl, mg/l =
Fraction = 5.80 / 6.21 = 0.934 10,000(WgtNaCl)(BrineSG)
New NaClmud = 22,710 x .934 NaCl, mg/l = 10,000(5.82)(1.28)
= 21,211 mg/l = 74,496 mg/l
WgtCaCl = D) SULFIDES
100 x 93,206 This procedure is used to measure the
93,206 + 21,211 + 10,000(25.0) active soluble sulfides concentration
= 25.58% by weight in an oil-base mud.
WgtNaCl = Equipment
100 x 21,211 11. Complete Garrett Gas Train (GGT).
93,206 + 21,211 + 10,000(25.0) 12. H2S Dräger tubes (low range and
= 5.82% by weight high range).
NaClmax = 26.432 – 1.0472 x 25.58 + 13. Flowmeter.
7.98191 x 10–3 x 25.582 + 5.2238 x 14. Flexible tubing made of Latex rub-
10–5 x 25.583 = 5.74 ber or Tygon (plastic or equivalent).
Fraction = 5.74 / 5.82 = 0.986 15. Magnetic stirrer.
18. Calculate the CaCl2 concentration 16. Magnetic stirring bar (1⁄4 in. x
in parts per million (ppm) 1 in.).
CaCl2, ppm = 10,000 x Final WgtCaCl 17. Hypodermic syringe: 10-ml glass
CaCl2, ppm = 10,000 x 25.58 or plastic.
= 255,800 18. 2 molar citric acid/isopropyl
19. Calculate the NaCl concentration alcohol/demulsifier solution.
in parts per million a. 420 g (C6H8O7H2O) citric acid
NaCl, ppm = 10,000 x Final WgtNaCl dissolved into 1,000 ml deionized
NaCl, ppm = 10,000 x 5.82 = 58,200 water.
20. Calculate the density of the brine b. To this solution add 25 ml of
(BrineSG) where BrineSG = brine Dowell W-35 demulsifier from
density, S.G. Fann Instrument or equivalent
BrineSG = 0.99707 + (an asphalt dispersant chemical).
0.006504(WgtNaCl) + c. To this solution add 200 ml of
isopropyl alcohol.

CHAPTER
3 Testing
19. Defoamer: octanol (CAS # 111-87-5). Connect the rubber hose from
10. 25-ml graduated cylinder. chamber 3 to the Dräger tube.
11. Carrier gas — CO2 cartridges, DO NOT START GAS.
or preferably, nitrogen. Do Not 12. Draw into the syringe the whole
use N2O. mud sample volume plus 0.5 ml of
12. Sample injection tube: 6-in. (15.2- excess mud. The excess mud com-
mm) long PTFE (Teflon or equiva- pensates for the hold-up volume
lent) needle or equivalent. inside the injection tube.
Procedure 13. Insert the syringe into the dip
11. Start with a clean, dry Garrett tube, and using a rubber band,
Gas Train. secure the syringe plunger to the
12. Modify the Garrett Gas Train by dip tube. This will prevent the cit-
inserting the sample injection tube ric acid-defoamer mixture from
through the rubber septum so that traveling up the dip tube when
the bottom end of the dip tube is pressure is applied.
approximately 1⁄2 in. from the bot- 14. Gently flow gas through the disper-
tom of chamber 1. The dip tube is sion tube for 10 to 15 sec to purge
used so that the mud sample can air from the GGT. Regulate the
be injected directly into the citric flow of gas to avoid frothing of the
acid solution. solution in chamber 1. Check for
13. Arrange the magnetic stirrer and leaks and for proper operation of
stirring bar (in chamber 1) so that the flowmeter.
the bar will rotate freely. 15. Turn on the magnetic stirrer.
14. Install CO2 cartridge. Adjust speed so that a vortex is
15. Add 20 ml of 2 molar citric acid/ formed. Carefully lower the disper-
isopropyl/demulsifier solution to sion tube into the liquid to a point
chamber 1. just above the stirring bar.
16. Add 10 drops of octanol defoamer 16. Lower the injection tube so that the
to chamber 1. bottom is slightly below the disper-
17. Break tips of H2S Dräger tube and sion tube. This will allow the oil
insert into the Garrett Gas Train mud to be injected into the vortex.
holder on the extreme right side. 17. Slowly inject a measured amount**
The arrow indicating the gas flow (see Table 6 on page 3.38) of oil-base
should be pointing down. Place mud into chamber 1 through the
an O-ring on the Dräger tube. injection tube. Increase the speed of
18. Insert the flowmeter in the other the stirring bar to improve disper-
holder with the air flow arrow sion and to prevent oil mud from
pointing up. Place an O-ring on sticking to the walls. Continue to
the flowmeter. stir for 1 min.
19. Install the top of the Garrett Gas 18. Use a rubber band to secure the
Train and tighten all screws to seal. plunger of the syringe in place.
10. Adjust the dispersion tube so that Restart gas flow. Adjust the rate so
the tube is positioned above the that the flowmeter shows between
liquid level. 200 and 400 ml/min by keeping
11. Connect the rubber hose from the the flowmeter ball between the red
regulator to the dispersion tube. marks on the flowmeter.

CHAPTER
3 Testing
19. Observe changes in appearance of and then with water. Occasionally,

the Dräger tube. Note and record the dispersion tube may require
the maximum distinct darkened soaking in an acid to remove
length (in units marked on the calcium carbonate deposits. The
tube) before the front starts to organic solvents can crack the
“feather” or smear. Continue flow- lucite body of the GGT.
ing for a total of 15 min, a second Using the sample volume, the
gas cartridge may be required. Dräger tube darkened length, and
20. Clean the GGT immediately after the Dräger tube factor, calculate
use to minimize deterioration of sulfides in the sample.
the plastic. Clean the chambers GGT sulfides (mg/l) =
and passages with warm water and darkened length x tube factor
a mild detergent. Wash the disper-
sample volume (ml)
sion tube and injection tube with
an organic solvent such as acetone
Pilot Testing
In drilling fluid engineering work, the specific gravity of the fluid must
calculations are based upon the oil- be taken into account. For example,
field barrel. The oilfield barrel con- if a fluid has a specific gravity of 1.2,
tains 42 U.S. gal. Mud treatments are then only 0.83 ml will be needed for
generally made by adding a certain 1 g or 1 lb/bbl. The specific gravities
number of pounds (or fractions of of most materials are contained either
a pound) of material to the oilfield in Product Bulletins or the Material
barrel of mud. Safety Data Sheets.
For pilot test and laboratory work, Purpose
an oilfield barrel would be difficult to By using these reduced quantities of
handle. It is much more convenient materials several possible treatments
to work with a much smaller sample can be tested economically prior to
of fluid. Instead of working with a bar- treating the mud system as a whole.
rel of fluid one works with a “barrel This procedure is useful not only when
equivalent.” A barrel equivalent con- contamination arises, but also to eval-
tains 350 ml of fluid. This representa- uate treatments when an alteration of
tive amount for one barrel is obtained fluid properties is planned. It should
as follows: be noted chemical solubility and effec-
An oilfield barrel has a volume of tiveness may be enhanced by actual
42 U.S. gal. It would hold 350 pounds circulation conditions, i.e. temperature
of fresh water. Three hundred and and pressure. Therefore, it is advisable
fifty g of water would occupy a volume to stage the addition of chemical treat-
of 350 ml in the metric system. Thus, ment over two or more circulations to
350 ml can represent the 42 U.S. gal, avoid over-treatment. For example, 60
or oilfield barrel. If 1 g of a material is to 70% of the planned addition can be
added to this barrel equivalent, this made on one circulation and adjust-
would be the same as adding 1 lb of ments to the total amounts made prior
material to an oilfield barrel. If a liq- to adding the remaining chemicals.
uid is added to the final barrel, then Additions of lime to a clay-base mud

CHAPTER
3 Testing
are an example of a treatment difficult 2. Suitability for existing mud system

to pilot test without heat aging to and hole conditions, i.e. temperature
simulate downhole conditions. and salinity.
Equipment 3. Effectiveness relative to cost.
1. Balance accurate to 0.1 g. To more closely simulate bottom-hole
2. Hamilton Beach-type mixer or conditions samples are frequently heat
equivalent. aged at bottom-hole temperatures and
3. Samples of chemicals to be tested for time periods equivalent to antici-
(preferably obtained at the rig site). pated periods of no circulation. Most
4. Equipment to perform mud check. ovens used for this procedure allow the
5. Roller oven complete with aging cell to remain either static, roll or rotate
cells if the sample is to be heat aged. during aging. If the sample is to be heat
Procedure aged certain safety precautions must be
A sample of the fluid to be tested is observed (some guidelines taken from
collected and a base mud check run API Recommended Practice 13I, Fifth
and recorded. Based on the properties Edition, Supplement 1, July 1996).
recorded a judgement is made as to 1. Use only cells constructed of stainless
the type and amounts of treatment steel (303, 304 or 316, but not 314)
chemicals necessary to achieve the unless testing for prolonged periods
desired results. of time at elevated salinities. In that
Since the agitation imparted to the case the use of premium metal cells is
mud sample during the addition of advised, i.e. IconelT 600, HastalloyT C
treating chemicals can by itself alter or IncolloyT 825. These types of cells
the fluids properties, a “control” sam- do have a lower strength rating than
ple should be stirred for an equivalent the stainless cells. Any aging cell used
amount of time and the properties must be constructed to exceed the
recorded for comparison. temperature and pressure require-
Careful notation of the order of addi- ments of the test.
tion of all treatments should be kept. 2. A major consideration is not to
The reasoning for this is most evident overfill the aging cells. When filling
by the example of the properties dis- the cells an adequate space must be
played by fluid samples containing left to allow expansion of the test
water, bentonite and NaCl. If the salt is fluid. In general no more than 1 bbl
added first hydration of the bentonite equivalent should be added to an
is suppressed and the fluid properties individual cell. This will generally
are markedly different. Whether the leave a gap of ±2 in.
chemicals are added “dry” or in solu- 3. Upon the cells removal from the
tion will also effect results. For this rea- oven the cell should be allowed to
son chemicals used in pilot testing cool to room temperature. If you
should be added in their normal order cannot touch the cell barehanded
of addition to the mud system and in it is not cool enough, even when
the same physical state. cool to the touch the interior may
Which additives to test is governed still be hot. REMEMBER: THE CELL
by the following criteria: CONTAINS PRESSURE GENERATED
1. Availability. BY THE VOLUME EXPANSION OF
THE FLUID!

CHAPTER
3 Testing
4. After cooling, the top of the cell can The M-I program MUDCALC gener-
be SLOWLY unscrewed, be sure any ates a list showing the quantities of
remaining pressure is released prior materials needed to mix pilot tests at
to the final turns. If you can safely specified concentrations. The specific
wiggle the top without hearing an gravities of many products are con-
escape of pressure you are probably tained within the program. You will
safe, however NEVER lean over the need to have the specific gravity of
top of a cell while opening. Any any product not listed.
remaining pressure can propel the To assist in pilot testing some approx-
top at gun-barrel speeds and with imate spoon weights for common oil-
the same effects. field products are listed (see Table 7).
It is preferred to accurately weigh the
products to 0.10 g whenever possible.
The spoon weights can be inaccurate
depending on the physical condition
of the sample.
Figure 22: Hot roll oven.

CHAPTER
3 Testing
1 1
Specific ⁄4 ⁄2 1 1
Product Gravity Teaspoon Teaspoon Teaspoon Tablespoon
Benex 1.2 0.90 1.80 3.60 10.80
Caustic soda 2.13 1.25 2.50 5.00 15.00
CMC 1.60 0.50 1.10 2.30 6.60
Desco 1.60 0.75 1.50 3.00 9.60
Diaseal M >2.0 0.80 1.60 3.20 12.60
Drispac 1.50-1.60 0.60 1.20 2.40 7.60
DUO-VIST 1.5 0.75 1.50 3.00 10.00
FLOXITE 1.4 0.40 1.00 2.00 6.50
GELEXT 1.2 1.00 1.75 3.50 11.00
Gypsum 2.32 1.30 2.30 4.90 12.60
Ironite sponge 4.30 1.50 3.50 8.00 25.00
KOH 2.04 1.00 2.50 5.00 15.00
KWIK-THIKT 2.3-2.6 1.00 2.00 4.00 12.00
Lime 2.20 0.60 1.30 2.40 7.70
Lo Loss 1.5 0.50 1.50 3.00 9.00
LO-WATEE 2.8 1.00 2.25 4.50 13.00
MF-1 1.2 0.50 1.50 3.00 10.00
M-I BART 4.20 2.08 4.17 8.33 25.00
Mica 2.75 0.50 0.80 2.00 5.80
Mixical 2.70 1.00 2.50 5.00 15.00
M-I GELT 2.30-2.60 0.98 1.95 2.90 6.70
MY-LO-JELE 1.45 0.63 1.25 2.50 7.50
Phos 2.5 1.00 3.00 6.00 20.00
POLYPACT R 1.5-1.6 0.50 1.00 2.00 8.00
Potassium chloride 1.98 1.90 3.10 6.10 19.10
Quebracho 1.10-1.40 1.00 2.00 4.00 12.00
RESINEXT 1.65 0.75 1.50 3.00 10.50
Salt 2.16 1.50 3.00 6.00 18.00
SALT GELT 2.20-2.40 0.70 1.50 3.00 8.80
SAPP 1.90 1.15 2.30 4.60 13.80
Soda ash 2.51 1.60 3.00 6.00 17.80
Sodium bicarbonate 2.16 0.72 1.45 2.90 8.70
Soltex 1.2-1.5 0.50 1.00 2.00 6.00
SP-101T 1.05 0.75 1.50 3.00 10.00
SPERSENEE 1.20 0.50 1.00 2.00 6.00
Starch 1.50 0.60 1.00 2.00 5.80
TANNATHINT 1.60 0.85 1.70 3.40 10.20
THERMPACT 1.50 0.50 1.00 2.00 8.00
VG-69T 1.57 1.00 2.00 3.00 9.00
XCD polymer 1.5 1.00 1.90 3.60 10.70
XP-20KE 1.83 1.17 2.33 4.67 14.00
Table 7: Approximate spoon weights for common oilfield products.

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CHAPTER

Water-Mud Testing ............................................................................................. 3.3

Testing 3.1 Revision No: A-1 / Revision Date: 02·28·01

Section 12. Permeability Plugging Test Procedure ........................................... 3.43

Oil-Mud Testing (Including Diesel Oil,

Pilot Testing ............................................................................................................... 3.63

Testing 3.2 Revision No: A-0 / Revision Date: 03·31·98

Section 1. Density of Fluid (Mud Weight)

Testing 3.3 Revision No: A-0 / Revision Date: 03·31·98

4. Place the balance arm on the base, Mud gradient:

Testing 3.4 Revision No: A-0 / Revision Date: 03·31·98

2. Immediately remove the finger Torsion spring constant

Testing 3.5 Revision No: A-0 / Revision Date: 03·31·98

1) PROCEDURE FOR APPARENT VISCOSITY, 2) PROCEDURE FOR GEL

u300 NOTE: Never immerse meter in water.

Figure 4: Typical flow curve for a drilling mud.

Testing 3.6 Revision No: A-0 / Revision Date: 03·31·98

Testing 3.7 Revision No: A-0 / Revision Date: 03·31·98

5. Open the inlet valve applying pres-

Testing 3.8 Revision No: A-0 / Revision Date: 03·31·98

Testing 3.9 Revision No: A-0 / Revision Date: 03·31·98

15. Seat lid properly, align and tighten

Testing 3.10 Revision No: A-0 / Revision Date: 03·31·98

Disassemble after there is no remain- 2. Temperatures over 350 to 400°F

Section 4. Sand Content

Testing 3.11 Revision No: A-0 / Revision Date: 03·31·98

Section 5. Liquid and Solid Content

Testing 3.12 Revision No: A-0 / Revision Date: 03·31·98

2. Four measurements are taken: 2. Disassemble retort and add mud to

#2 = 348.31 – 317.45 = 30.86 g of mud

Testing 3.13 Revision No: A-0 / Revision Date: 03·31·98

Testing 3.14 Revision No: A-0 / Revision Date: 03·31·98

D) FLOCCULENT EFFICIENCY TEST flocculent would not be required at

Section 6. Hydrogen Ion Concentration (pH)

Testing 3.15 Revision No: A-0 / Revision Date: 03·31·98

B) PH METER 13. Clean electrodes-wash with

Testing 3.16 Revision No: A-0 / Revision Date: 03·31·98

as indicated by slow response, drift-

Section 7. Chemical Analysis of Water-Base Drilling Fluids

A) ALKALINITY (Pf, Mf, Pm AND 1) PROCEDURE FOR FILTRATE ALKALINITY

Testing 3.17 Revision No: A-0 / Revision Date: 03·31·98

Testing 3.18 Revision No: A-0 / Revision Date: 03·31·98

Testing 3.19 Revision No: A-0 / Revision Date: 03·31·98

Attach Dräger hand pump to other

flow. Table 3: Sample volumes and tube factor

It can cause an explosion if misused in

Salt (mg/l x 1,000)

nificant in areas where salt can conta- 5

Equipment Figure 14: Salt milligrams per liter vs.

Testing 3.21 Revision No: A-0 / Revision Date: 03·31·98

D) CALCIUM - QUALITATIVE E) TOTAL HARDNESS

Testing 3.22 Revision No: A-0 / Revision Date: 03·31·98

3. Add 1 ml of strong buffer solution 2) CALCIUM AND MAGNESIUM SEPARATELY

determine total hardness. The follow- QUANTITATIVE

Testing 3.23 Revision No: A-0 / Revision Date: 03·31·98

19. Beaker, 100-ml. 3. Add 1 ml of acetic acid and mix.

Testing 3.24 Revision No: A-0 / Revision Date: 03·31·98

Calculations 13. Calmagite Indicator.

Testing 3.25 Revision No: A-0 / Revision Date: 03·31·98

13. Record the number of ml of to determine sample size. Be sure to

4. Bromophenol blue indicator. ml of QAS x 4

two 5-ml and two 10-ml. ml of filtrate*

Testing 3.26 Revision No: A-0 / Revision Date: 03·31·98