Chapter 09 Procedures and Laboratory Equipment (

WATER-BASED DRILLING
PROCEDURES AND FLUIDS

LABORATORY
EQUIPMENT
(NON INHIBITING)
Well Area Operations

Agip KCO Drilling Supervisors Training Course
Drilling Muds RPW2021A 1
INTRODUCTION
• The American Petroleum Institute (API) recommends standardized methods for

laboratory and rig site tests which can be found in their publications.
• Recommended Practice: Standard Procedure for Field Testing Water-Based (Oil-

Based)
• Drilling Fluids, API RP 13B-1, 13 B2.

FLUID DENSITY (or MUD DENSITY)
INSTRUMENTS
The density, commonly called “mud weight” is checked with a mud balance whose
precision has a margin of error of 0.1 lb/gal. (10 gr/l).
The density is defined as weight per unit of volume.
The weight of mud may be expressed as density in: lb/gal or lb/ft3 or Specific Gravity
(SG)
lb/gal lb/ft 3 g kg
SG = or or or
8.345 62.3 cm3 litre

MUD BALANCE
Description
Balance for mud

CALIBRATION
9 Fill the cup with pure or distilled water.
9 Put the graduated bar of the balance down with care so that it is in equilibrium on
the fulcrum.
9 The level-bubble should be centred when the reader is set on 1 g./cm2 or 8.33
lb/gal. If not, it will be necessary to carry out an adjustment on the calibration
screw situated at the end of the same bar.

PROCEDURE
1. Fill the vessel with a sample of mud to check its weight.
2. Put the cap on again, rotate it several times to ensure that no solids are in its seat.
3. Rinse all and dry with a cloth.
4. Put the graduated bar of the balance down with care in equilibrium on the fulcrum.
5. Move the slider until the bubble of air is in the centre.
6. Read, near the cursor, the weight (or density) of the mud.
7. Write the weight, according to the system of measure desired, both in lb/gal, lb/ft3,
psi/1,000 ft of depth or Specific Gravity (SG).
8. If the balance in use does not have the system desired, the following equations
may be used.

MUD GRADIENT
psi/ft = 0.052 x lb/gal

= 0.4333 x SG
= 0.00695 x lb/ft3
kg/cm2/m = SG / 10
SG a 60°F (15.6°C) = (141.5) / (131.5 + °API)
Where: °API = American Petroleum Institute gravity

VISCOSITY
INSTRUMENTS
The Marsh Funnel is used in the rig site to measure the viscosity. The Fann V-G
viscosimeter is used when complete information on rheology is necessary(Plastic
viscosity, yield point and gels).
Marsh Funnel and graduated cup

MARSH FUNNEL
Description
The Marsh Funnel is 6 inch. In diameter at the top and 12 inch long. At the bottom is has
a 2 inch smooth-bore tube having an insider diameter of 3/16 inch.
Calibration
Fill the funnel till the bottom of the screen (1,500 cm3) with fresh water at
70±5°F. The time to flow of 1 qt (946 ml) should be 26 sec ±0.5 sec.

MARSH FUNNEL
Procedure
9 Collect a fresh mud sample
9 Hold the funnel erect with a finger over the outlet tube, and pour the mud into the
funnel through the screen until the mud level reaches the bottom of the screen (The
screen will filter out the larger particles that could clog the outlet tube)
9 Quickly remove the finger from the outlet tube, and at the same time, begin timing the
mud outflow
9 Allow one quart of gallon (946 cc) of mud to drain from the Marsh Funnel into a
graduated container
9 Record the number of seconds it takes for the quart of mud to flow out of the funnel,
and report this value as the Marsh Funnel Viscosity. Also record the temperature of
the mud sample in degrees F or C.

ROTATIONAL VISCOSIMETER
With a Rotational Viscosimeter it is possible to

measure the rate/shear stress of a drilling fluid
and you can calculate the Bingham PV and YP
parameters. With the same data it is possible to
use other rheological models. The Rotational
Viscosimeter is also used to measure the
thyxotropic properties and gel strength
Description
The Rotational Viscosimeter offers a direct

reading and functions electrically.

SPECIFICATIONS: DIRECT READING
VISCOSIMETER
Rotor sleeve (external cylinder)

Internal diameter 1.450 in. (36.83 mm)
Total length 3.425 in. (87.00 mm)
Reference line 2.30 in. (58.4 mm) above the bottom of the cylinder.
Two rows of 1.8-in. (3.18-mm) holes spaced of 120 degrees (2.09 radiants)
around the rotor just below the reference line.
Bob (internal cylinder)

Diameter 1.358 in. (34.49 mm)
Cylinder length 1.496 in. (38.00 mm)
The BOB is closed with a flat base.

VISCOSIMETER
Constant spring torsion

386 dyne-cm/degrees defletion
High 600 RPM

Rotor Speeds:
Low 300 RPM

VISCOSIMETER
The following types of viscosimeters are normally used to test the fluids:
¾A handle viscosimeter has a speed of 300 and 600 RPM. A control situated at the point
of the speed change lever is used to determine the gel strength.
¾The electrical motor type (12-volt) has a speed of 300 and 600 RPM. A “governor-
release” type switch allows a strong agitation before the determination of the
measurement, then a hand wheel is used to determine the gel strength.
¾The electrical motor type, 115-volt, allows two synchronized speeds in the range
between 600, 300, 200, 100, 6 and 3 RPM. The speed of 3-RPM is used to determine
the gel strength.
¾At variable speed (115- or 240-volt with electrical motor) it allows variable speed from
625 to 1 RPM. The speed of 3-RPM is used to determine the gel strength.

PROCEDURE TO DETERMINE APPARENT
VISCOSITY, PLASTIC VISCOSITY AND YIELD POINT
¾ Shake the sample then pour it, into the thermocup until the level reaches the
appropriate line of the rotor.
¾ Increase or decrease the temperature of the sample to 59°C (120°F). Stir slowly
during the calibration of the temperature.
¾ Start the motor rotating with the knob on high speed and the gear level at the
bottom. Wait for a stabilized reading and report the reading at 600 RPM. Change
the ratio only when the motor is working.
¾ Select a rotation speed of 300-RPM. When the value is stabilized report the
reading at 300-RPM.

PROCEDURE TO DETERMINE APPARENT
VISCOSITY, PLASTIC VISCOSITY AND YIELD POINT
• Plastic Viscosity in centipoise = Reading at 600 RPM – Reading at 300 RPM (see
figure below)
• Yield Point in lb/100 ft2 = reading at 300 RPM less the plastic viscosity in
centipoise.
• Apparent Viscosity in centipoise = reading at 600 RPM divided by 2.
Typical “flow curve” of a drilling fluid.

PROCEDURE TO DETERMINE THE GEL
STRENGTH (AT 10” AND AT 10’)
¾ Shake the sample of mud at 600 RPM for approximately 15 sec and raise the gear
lever to the neutral position.
¾ Step 1: stop the motor and wait for 10” sec.
¾ Step 2: move the switch to low speed and report the unit of maximum deflection in
lb/100 ft2. If the indication of the instrument should not return to zero do not
reposition it.
¾ Repeat step 1 and 2, wait 10’ minutes then position the lever on low speed and
read the unit of maximum deflection. Report the temperature measured.

FILTRATION
DESCRIPTION
The filtration, or capacity of a mud to constitute a filter cake is determined by the filter
press. The test defines the Ratio with which a fluid is forced through the filter press.
This API Fluid Loss test must be carried out in specific conditions of duration,
temperature and pressure that according to the API Recommended Practice are
surface temperature, 100 psi and recorded as the number of millimeters lost in 30
minutes.

INSTRUMENTS
Cell
Graduated
cylinder
Carbon dioxide
Example of Filter Press
cartridges

API FLUID LOSS
Procedure
1. Pressure availability at 100 psi with gas or air.(7 Kg/cm2).

2. Remove the cap from the bottom of the cleaned and dried cell. Install the O-ring to
check that its seat is not damaged, then turn the cell upside down for the filling.
Any mechanical imperfection can compromise the seal. Close the inlet hole with a
finger.
3. Fill the cell with mud up to ¼ inch from the housing of the O-ring. Put the filter
paper (Whatman No. 50 or equivalent) over the O ring. Put the cap on the filter
paper with its flanges between those of the cell, then turn in a clockwise direction
and close by hand. Turn the cell upside down and insert the cell body into the
bottom of the mud chamber of the filter press and turn in either direction to lock
the closure.

API FLUID LOSS
4. Put a graduated cylinder under the drain tube.
5. Open the valve to pressurize the cell. You will immediately notice a fluctuation of
the needle of the manometer which will indicate higher pressures during the
pressurization and then, it stabilizes at 100 psi.
6. The API duration for this test is 30 minutes. When the test is finished, close the
valve to stop the pressure at the source. The purge will occur automatically.
Remove the cell.

API FLUID LOSS
7. Report the fluid loss in millilitres.
8. Disassemble the cell, remove the mud and carefully remove the filter of paper in
order to avoid any minimum damaging to the mud cake. Wash the cake and
remove the mud in excess. Measure the thickness of the cake and report it in 32
nds of an inch.

HIGH-TEMPERATURE, HIGH-PRESSURE (HTHP)
FILTRATION (High Pressure High Temperature)
HTHP Filter Press
MB style (API #II) HTHP filter press
Description
The instrument consists of a heating
jacket with thermostat, cell plate
assembly, primary pressure assembly
and back-pressure receiver. The
capacity of the mud cell is 160 ml with
a filter area of 3.5 in.2.
Filtrate receiver holds 15 ml, and up to
100 psi backpressure can use a glass
tube. If a higher back pressure is to be
used, a stainless-steel tube should
replace the glass.
A routine test can be conducted at
300°F and 500 psi differential pressure.
High-temperature fluid loss is recorded
as double the number of milliliters lost
in 30 min.

Procedure
1. Turn on the heating and wait for the instrument to reach the pre-heating
temperature. Put the thermometer in its housing and control the thermostat to
reach a temperature higher than the desired one of 10 °F.
2. Close the inlet valve of the cell and invert the cell.
3. Take the mud from the flow line. Pour it inside the vessel up to 0.2” below the
housing of the O-ring and wait for the expansion.
4. Put a filter of paper in the appropriate housing and put over it the O-ring. Use a
Watman filter No. 50 or equivalent.
5. Put the cover above the filter of paper and block it.
6. Shut the caps with strength and close the bleeding valve.

7. With the cap of the cell at the bottom, put the cell inside the heater making sure
that all valves are closed. Transfer the thermometer to its location.
8. Install the cylinder of CO2 in its seat and turn it clockwise until the cover is opened.
The controller and the purge valve must be closed.
9. Keeping the lock ring raised, insert the primary unit of pressure in the upper
housing, and turn the lock ring to close.
10. Introduce a pressure of 100 psi against the valve, then open it to pressurize the
unit. This pressure will minimize the boiling during the heating of the sample.
11. Always use a container to prevent the vaporization of the filtrate if the test
temperature will reach or exceed the boiling temperature. Install and activate the
cylinder of CO2 in the purge unit.
12. Install the purge unit in the proper housing.

13. Apply a pressure of 100 psi. at the lower unit while the valve is still closed.
14. Once you have reached the desired temperature (300°F), as indicated by the
thermometer, increase the pressure of the controller in the upper cell from 100 to
600 psi to make the pressure increase, keeping 100 psi with the lower controller.
Open the lower cell valve by one turn and start the test.
15. Keep a pressure of 100 psi on the receiver during the test. If the pressure raises,
discharge some of the filtrate and keep a differential of 500 psi. Keep the
temperature at ±5°F.

16. After 30 min., close the valve of the lower cell and then the higher one.
17. Loosen either T-screws in the controller and discharge the pressure from either
controllers.
18. Discharge the filtrate in the graduated cylinder and read the volume. Double the
reading in the ratio. Remove the receiver.

19. Disconnect the primary unit of pressure raising the blocking ring and taking off the
unit. CAUTION: The cell is pressurized.
20. Hold the cell erect and leave cooling at ambient temperature, then discharge the
pressure; the mud must not pass through the valve.
21. Invert the cell, then loosen the screen of the cup. (If necessary, use an hexagonal
key) and disassemble. Clean and dry the various parts.
22. Visually observe and note the condition of the filter cake. It can be measured in
1/32 of an inch.

API #I Filterpress HTHP
Tests at 300°F (149°C) or lower temperatures
Vapours pressure and expansion of the water volume between 212° and 450°F
Coefficient of the Expansion Volume of External pressure

Treating temperature Water vapours pressure
water at a Saturation Pressure suggested
°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 1104 160
400 205 1703 247 1.16 1898 275
450 232 2917 422 1.21 3105 450

API #I Filterpress HTHP
Tests at 300°F (149°C) or lower temperatures

TEST AT TEMPERATURE BETWEEN 300 AND
400°F (149 to 233°C)
The same procedures are used, except the following cases, where the 500-ml cell is
suggested, manifold pressurization with azote:
1. During the heating of the sample, pressurize either units with 450 psi. At the
beginning of the test, the higher pressure raises at 950 psi while the lower pressure
is kept at 450 psi.
2. With temperatures between 350 and 400°F, a porous stainless steel disk (Dynalloy
X5 or equivalent) is preferred . (see API RP 13B-1 and 13B-2).
3. Heating time should not exceed 1 hour.

FILTER-CAKE COMPRESSIBILITY
For this test, the same procedure compared to 300°F (149°C) is applied, but there’s
a difference infact, 200 psi are applied to the cell and 100 psi to the receiver at the
bottom. The differential values regarding 100 and 500 psi are then compared.

SAND CONTENT
INSTRUMENTS
KIT FOR SAND CONTENT
The Sand Content Kit determines the volume percent of sand-sized particles in the
drilling fluid. API defines sand-sized particles as any material larger than 74 microns
(200 mesh) in size. This test can be performed on low solids fluids as well as on
weighted fluids. The kit consists of a glass tube graduated to read percent (%) by
volume, a funnel, and a 200-mesh sieve contained in a cylindrical-shaped holder.

SAND CONTENT
Procedure
1. Fill the glass vessel to the indicated mark with mud. Add water to the next mark.
Close the mouth of the vessel and shake vigorously
2. Pour the mixture onto the screen, add more water to the vessel shake and again
pour onto the screen. Repeat until water will be clear. Wash the sand remained on
the screen
3. Put the funnel over the mouth of the vessel. Insert the tip of the funnel into the
mouth of the glass vessel. Wash the sand on the screen by spraying a fine spray
of water. Allow the sand to settle, from the graduate on the tube, read the volume
percent of the sand.

SAND CONTENT KIT
200 Mesh
screen
"Mud"
line
Funnel
"Water"
line
Sand %
graduation
Elutriometer

SOLIDS AND LIQUIDS CONTENT
INSTRUMENTS
The distillation of the mud through the heating can define the quantity of liquids and
solids in the mud. A sample of mud (distillers available 10, 20 or 50 cm3), is placed
in the cup and it is heated until the liquid components have been vaporized. Then,
they are pressed through a condenser and collected in a percent graduated cylinder.
The volume of liquid (oil and water) is measured directly in percent. The solids, both
suspended and dissolved, are determined by subtracting from 100%. The distiller is
also called Ministil and/or Retort.

KIT FOR OIL AND MUD DISTILLATION
Retort Condenser
Retort Stem
Retort Cody
Retort Assembly
Steel Wool Condenser
Discharge
Lid
Retort Cup Liquid

Receiver

DISTILLER DESCRIPTION
Procedure
1. Allow the mud to cool down to ambient temperature.
2. Disassemble the distiller and lubricate the threads of the cup with grease for high
temperature. Fill in the sample cup with the mud till the edge. Put on the cap, make
a firm rotation and let pour out the fluid in excess. The correct volume of mud, which
can be 10, 20 or 50 cm3, is defined. Dry any possible trace of mud.

3. Fill the upper expansion chamber with a steel wool which will trap the boiling
solids. Hold all erect so that the mud cannot flow into the drain tube.
4. Insert, or screw the drain tube in the hole situated at the end of the
condenser. The graduated cylinder, which is calibrated in order to allow the
reading of the percentage, will be then arranged in the condenser.
5. Connect to the electrical network and keep the current till the completion of the
distillation. This could require 25 minutes, according to the characteristics of
the oil, water and the content of solids.

6. Allow the distillate to cool down to ambient temperature
7. Read the % of water, oil and solids. A couple of drops of aerosol solution will help
the definition of the oil-water interface, after the reading of the solids percentage.
8. Once you have finished the test, cool the distiller then clean and dry it .
9. Run a pipe cleaner through condenser hole and retort drain tube to maintain full
openings.

METHYLENE BLUE CAPACITY
It is the field procedure to define cation exchange capacity (for Shales)
Equipment
1. Syringe, 3 cm3, burette 10 cm3.

2. Micropipette, 0.5- cm3.
3. Erlenmeyer flask (graduated), 250- cm3 with a gum plug.
4. Burette or pipette, 10- cm3.
5. Graduated cylinder, 50- cm3.
6. Mixer vane.
7. Hot plate.
8. Filter paper: diametre 11 cm, Whatman No. 1 or equivalent.

Reagents
1. Methylene blue solution:
1 cm3 = 0.01 milliequivalents
3.74 g of methylene blue, USP degree
(C16H18N3SCl•3H2O) per litre.
2. Hydrogen peroxide, solution at 3%.
3. Sulphuric acid solution 5 N.

PROCEDURE
1) Add 2 ml of muds to 10 ml of water in the E. Flask. Add 15 ml of 3% hydr.
Peroxide and 0.5 ml of 5N sulfuric acid solution and mix. Boil gently for 10 min.
(this initial treatment is to remove the organic materials like CMC,
lignosulfonate…). Dilute to about 50 ml with water.
2) Add Methylene Blue Solution 0,5 ml at time, and shake for 30 sec. after each
addition. While the solids are still suspended, remove 1 drop from the flask with a
glass rod and place on filter paper. The end point of the titration is needed when
the dye appears as a greenish-blue ring surrounding the dyed solids.
3) Record the ml of methylene blue solution used.
MBC of mud in lbs/bbl = (cm3 of methylene blue/cm3 of mud used) x 5
MBC of mud in kg/m3 (cm2 of methylene blue/cm3 of mud used) x 14

HYDROGEN IONS CONCENTRATION (pH)
AIM
Mud (or filtrate) pH surveys and pH adjustments, are fundamental in order to control
the drilling fluid. Interactions of the clay, solubility of the various components and the
effectiveness of the additives depend on the pH, as well as the control of the
corrosion caused by acids and sulphates. Th pH is used to describe the acidity or
basicity of solutions. The pH value is defined as the negative logarithm of the
hydrogen ion concentration: pH = - log [H+].
Low pH value corresponds to acids and high pH values correspond to basic solution.
The range of pH is 0 to 14.
7 is neutral (water).

pH INDICATOR STICKS
Description
These pH indicators sticks are coated with indicators whose colour is dependent on the
ph of the fluid in which the stick is placed. Standard colour charts are supplied for
comparison with the test stick, allowing estimation of pH to 0.5 pH units. (from 0 to 14).

pH METERS
Description
The pH meter, equipped with a glass electronic electrode is the recommended method
for measuring the pH in drilling fluids. Surveys are highly accurate, easy and auto-
adapting to the temperature variations.

pH METERS Equipment
• A portable pH meters consists of a

probe and an electronic indicator. The
probe consists of:
• A glass Electrode
• An Electro standard reference
• Temperature detector (optional)
Portable pH meters

pH METER
The recommended procedure to detect the pH is as follows:
Measurements consist of:
9 Instrument calibration.
9 pH survey from a sample.
9 Cleaning and storage of the probe.

CHEMICAL ANALYSIS OF WATER
IN THE MUD
INTRODUCTION
Alkalinity Titrations define OH-, HCO3- and CO3-- concentrations, by measuring the
amount of acid required to reduce the pH.
Phenolphtalein Alkalinity (P) is reported as the number of millimeters of 0.02 N H2SO4

required to titrate a ml of filtrate (Pf) or mud (Pm), reducing the pH at 8.3.
The methyl orange filtrate alkalinity Mf measures the acid (H2SO4) required to reduce the
pH at 4.3.

CHEMICAL ANALYSIS OF WATER IN THE MUD
Alkalinity (Pf, Pm, Mf and lime content)
Equipment
The following materials and products are necessary in order to define the alkalinity of
the mud and lime:
1. Standard acid solution, 0.02 N (N/50); nitric or sulphuric acid (as an alternative, It is
also possible to use an acid solution 0.1N(N/10). However, it must be converted to
the equivalent of ml 0.02 N multiplied 5).
2. Phenolphtalein indicator solution.
3. Methyl orange indicator solution.

CHEMICAL ANALYSIS OF WATER
IN THE MUD
4. Vessel for titration, from 100 to 150 cm3, preferably white.
5. Graduated pipettes: one 1 cm3 and one 10 cm3.
6. Stirring rod.
7. One syringe from 1 cm3.
8. pH meter with glass electrode. (optional but suggested)

PROCEDURE FOR THE ALKALINITY OF THE FILTRATE
(PF AND MF)
1. Measure 1 cm3 of filtrate in the vessel for titration, then add 5 cm3 of deionized
water (distilled water).
2. Add 2 or more drops of phenolphtalein indicator. The solution turns pink.
3. Add acid N/50 drop by drop while stirring, until the pink colour just disappears. If
the colour of the sample cannot be defined because of its intensity, the end point
must be surveyed when the pH drops to 8.3, as measured with the pH meter. (The
sample can be diluted with distilled water.)
4. Report the Phenolphtalein Alkalinity of the filtrate, Pf, as the number of cm3 of
0.02 of N acid required for every cm3 of filtrate to reach the end point.

PROCEDURE FOR THE ALKALINITY
OF THE FILTRATE (Pf and Mf)
5. To the same sample used to measure the Pf, add 3 to 4 drops of Methyl orange.
The reaction will give a green colour
6. Titrate with 0.02 N acid until a yellow colour is obtained. This will happen when a
pH = 4.3. is reached
7. The Mf is reported as the number of millilitre of acid used for the Pf plus this last
titration.
Example:
If you use 0.5 cm3 of acid to titrate the final point of the phenolphtalein the Pf is 0.5.

PROCEDURE - MUD ALKALINITY (Pm)
1. Measure 1 cm3 of mud into the vessel using the syringe. Dilute the sample with 25
cm3 of distilled water. Add 5 drops of Phenolphtalein Indicator, and while stirring,
titrate with 0.02 of acid N or with 0.1 of acid N until the pink colour just disappears.
N/50 or N/10 Sulphuric acid.
2. If the intensity of the colour cannot define the change, the end-point is reported
when the pH drops at 8.3, as measured with pH meter.
3. Report the phenolphtalein alkalinity of the mud, Pm, as the number of cm3 of acid
0.02 N (N/50) required per cm3 of mud. If the acid 0.1 N is used, Pm = 5 x cm3 of
0.1 acid N for cm3 of mud.

PROCEDURE FOR LIME CONTENT
After having defined the Pf and Pm, determine the volume fraction of water in the mud,
Fw, using the value from retort test. Report the lime content of the mud in lb/bbl
calculated as follows:
Lime (lb/bbl) = 0.26 x (Pm – Fw x Pf)

CHLORIDES (Cl–)
Aim
Chloride test is very important in those areas where salt can contaminate the mud.
The content of the chloride ion is an excellent detector for example, when
stratigraphic levels of salt and salt water areas are crossed during the drilling,
Moreover, the chloride test check the quality of industrial water.

CHLORIDES (Cl–)
Equipment
The following equipment is required for the determination of the chloride ion
concentration in the filtrate.
1. Silver nitrate solution, 0.0282N or 0.282N (strong) AgNO3, in an opaque bottle.

Italy ENI : 0,1N and 1N.
2. Potassium Chromate indication solution.
3. Sulfuric or nitric acid 0.02.
4. Distilled water.
5. Two graduated pipettes: one 1- cm3 and one 10- cm3.
6. Titration dish from 100 to 150 cm3, preferably white.
7. Stirring rod

CHLORIDES (Cl–)
PROCEDURE
1. Measure 1 cm3 into the titration dish.
2. Add the amount of acid required in the Pf titration.
3. Add 25 ml of distilled water and 10 drops of potassium chromate solution. Stir

continuously and titrate with standard silver nitrate solution, drop by drop until the
colour changes from yellow to orange-red and persists for 1 minute.

CHLORIDES (Cl–)
4. Report the number of cm3 of silver nitrate solution needed to reach the colour
change point:
Cl– (mg/l) = cm3 of 0.0282 N silver nitrate x 1,000 / cm3 of filtrate if a concentrate
silver nitrate solution is used (0.282 N): Cl- (mg/l) = cm2 0.282 Silv. Nitr. X 10.000/cm3
of filtrate.
Any normal silver nitrate or 0,1N (frequent for ENI):
Cl– (mg/l) = (N x 35,000 x cm3 used) / (cm3 of the sample filtrate)

CHLORIDES TITRATION
Chlorides Titration
Chlorides (Cl-) – Tinge colour filtrates

Chemical
analysis Column 1 Column 2
Sample 1 cm3 filtrate 1 cm3 filtrate
Deionized water No 25-50 cm3

Buffer No No
Colour Indicator 2-3 Phenolphtalein drops 8-10 drops of Potassium Chromate

0.02 (N/50) 0.028N AgNO3
Titrate with: H2SO4 (sulphuric acid) or 0.282N AgNO3
(Titolatore)
* (silver nitrate)
Colour change Filtrate, from pink to original From Yellow to Red-Orange

Record No (cm3 of 0.0282 N AgNO3 x 1,000) / cm3 of filtrate
or
(cm3 of 0.282 N AgNO3 x 10,000 ) / cm3 of filtrate
*Chlorides : 10,000 mg/l

See col. 2 If < use: 0.0282 N AgNO3
Note:
If > use: 0.282 N AgNO3

CALCIUM - QUALITATIVE
Aim
When water has a high content of mineral salts in particular calcium and magnesium,
is called “hard water”. The evidence of hardness in water at home is the difficulty in
producing a lather with soap.
When the water used to mix the mud is hard, drilling clays have low yields. Bentonite
must be used in greater amount to make a satisfactory thixotropy.
It is often economical to treat the water to reduce the hardness.
Calcium may also arrive from drilling out cement or gypsum or anhydrite levels.
Calcium contamination can increase gels and filtrate valve. The high hardness in the
mud reduces the effectiveness of the majority of the polymeric products.

CALCIUM AND MAGNESIUM TOGETHER –
QUANTITATIVE
Equipment
1. Standard Versenate Solution (EDTA) 0.01 M (1 ml = 400 mg Ca++ or 1,000 mg

CaCO3).
2. Buffer Hardness Solution (ammonium hydroxide/ammonium chloride).
3. Versenate solution as hardness indicator (Clamagite Indicator Solution).
4. Titration dish, 100 to 150 cm3, preferably white.
5. Three graduated pipettes: 1 cm3 , 5 cm3 ,10 cm3.

QUANTITATIVE
7. Graduated Cylinder, 50 cm3.
8. Distilled water.
9. Stirring rod.
10. NaOH, 8N solution or KOH.
11. Calcon Indicator Calver II
12. Porcelain Spatula.
13. Masking Agent: tritalonamine mixture at 1:1:2

QUANTITATIVE
Procedure (total hardness)
Add 50 cm3 of deionized water to the titration dish; add 2 cm3 (20 drops) of
versenate buffer solution (base NH4OH).
Add 10 drops of Versenate Hardness Indicator Solution (nero eriocromo t). If

calcium and/or Magnesium is present in the deionized water, a wine red-colour will
develop otherwise the solution will keep the blue colour.
During the stirring titrate with standard versenate (EDTA) unitl the colour turns
from red-wine to blue. Do not pass the colour change point.
Note: The steps 1-3 remove hardness from deionized water.

QUANTITATIVE
Procedure (total hardness)
Add to the deionized water 1 cm3 of filtrate. If there’s calcium and/or magnesium
a red-wine colour will develop. During the stirring, titrate (drop by drop) until the
colour turns from red-wine to blue.
Note the number of cm3 of versenate used (if magnesium is measured according
to procedures report the value as “A” cm3.) and calculate the hardness in mg/l.
A = total hardness; B = calcium hardness ;A-B = magnesium hardness.

QUANTITATIVE
Calculation
Total Hardness as Ca++ (mg/l) = (cm3 versenate x 400) / (cm3 sample)
CaCO3 (mg/l) = (cm3 versenate x 1,000) / (cm3 sample)
Occasionally, the dark colour filtrate could not be easily visible at the end point as a
consequence, it is difficult to define the total hardness. For a better definition of the
end point, the following mehtod is suggested.

TOTAL HARDNESS TITRATION
Total Hardness Titration
Total Hardness
Chemical analysis Column 1 Column 2
Sample No 1 cm3 of filtrate
Deionized Water 50 cm3 No
Buffer 2 cm3 Buffer Versenate hardness No
Colour Indicator 10 gocce Versenate Hardness indicator No
Titrate with: Standard Versenate Standard Versenate
Red-wine to blue
Change Colour Do not pass the end point Wine-red colour to blue
(cm3 of versenate x 400)/ (cm3 of
Record No the sample)
Note: Pass to column 2


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WATER-BASED DRILLING

PROCEDURES AND FLUIDS

Well Area Operations

• The American Petroleum Institute (API) recommends standardized methods for

• Recommended Practice: Standard Procedure for Field Testing Water-Based (Oil-

• Drilling Fluids, API RP 13B-1, 13 B2.

Well Area Operations

The density is defined as weight per unit of volume.

Well Area Operations

Balance for mud

Well Area Operations

9 Fill the cup with pure or distilled water.

Well Area Operations

1. Fill the vessel with a sample of mud to check its weight.

3. Rinse all and dry with a cloth.

5. Move the slider until the bubble of air is in the centre.

Well Area Operations

psi/ft = 0.052 x lb/gal

Where: °API = American Petroleum Institute gravity

Well Area Operations

Marsh Funnel and graduated cup

Well Area Operations

Well Area Operations

9 Collect a fresh mud sample

Well Area Operations

With a Rotational Viscosimeter it is possible to

The Rotational Viscosimeter offers a direct

Well Area Operations

Rotor sleeve (external cylinder)

 Total length 3.425 in. (87.00 mm)

around the rotor just below the reference line.

Bob (internal cylinder)

 Cylinder length 1.496 in. (38.00 mm)

 The BOB is closed with a flat base.

Well Area Operations

Constant spring torsion

High 600 RPM

Well Area Operations

Well Area Operations

Well Area Operations

Typical “flow curve” of a drilling fluid.

Well Area Operations

¾ Step 1: stop the motor and wait for 10” sec.

Well Area Operations

Well Area Operations

Well Area Operations

1. Pressure availability at 100 psi with gas or air.(7 Kg/cm2).

Well Area Operations

4. Put a graduated cylinder under the drain tube.

Well Area Operations

7. Report the fluid loss in millilitres.

Well Area Operations

Well Area Operations

Well Area Operations

12. Install the purge unit in the proper housing.

Well Area Operations

Well Area Operations

Well Area Operations

Well Area Operations

Coefficient of the Expansion Volume of External 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

Total length 3.425 in. (87.00 mm)

Cylinder length 1.496 in. (38.00 mm)

The BOB is closed with a flat base.