ISO 10414-1:2001

Petroleum and natural gas industries - Field testing of drilling fluids - Part 1: Water-based fluids

Industries du pétrole et du gaz naturel — Essais in situ des fluides de forage — Partie 1: Fluides aqueux

General Information

• Status: Withdrawn
• Publication Date: 28-Mar-2001
• Withdrawal Date: 28-Mar-2001
• ICS: 75.180.10 - Exploratory, drilling and extraction equipment
• Technical Committee: ISO/TC 67/SC 3 - Drilling and completion fluids, well cements and treatment fluids
• Drafting Committee: ISO/TC 67/SC 3/WG 1 - Drilling, completion and workover fluids
• Current Stage: 9599 - Withdrawal of International Standard
• Start Date: 10-Mar-2008
• Completion Date: 13-Dec-2025

Relations

• Revised: ISO 10414-1:2008 - Petroleum and natural gas industries - Field testing of drilling fluids - Part 1: Water-based fluids
• Effective Date: 15-Apr-2008

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 10414-1
First edition
2001-03-15
Petroleum and natural gas industries —
Field testing of drilling fluids —
Part 1:
Water-based fluids
Industries du pétrole et du gaz naturel — Essais in situ des fluides de
forage —
Partie 1: Fluides aqueux
Reference number
©
ISO 2001
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ii © ISO 2001 – All rights reserved

Contents Page
Foreword.iv
Introduction.v
1 Scope .1
2 Term and definition .2
3 Abbreviated terms .2
4 Drilling fluid density (mud weight).2
5 Alternative drilling fluid density method.4
6 Viscosity and gel strength.6
7 Filtration.8
8 Water, oil and solids contents.12
9 Sand content .16
10 Methylene blue capacity .17
11 pH .20
12 Alkalinity and lime content .23
13 Chloride ion content.25
14 Total hardness as calcium.27
Annex A (informative) Chemical analysis of water-based drilling fluids.29
Annex B (informative) Shear strength measurement using shearometer tube .45
Annex C (informative) Resistivity .47
Annex D (informative) Removal of air or gas prior to testing.48
Annex E (informative) Drill pipe corrosion ring coupon .49
Annex F (informative) Sampling, inspection and rejection.52
Annex G (informative) Rig-site sampling.54
Annex H (informative) Calibration and verification of glassware, thermometers, viscometers, retort kit
cup and drilling fluid balances.57
Bibliography.62
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO
member bodies). The work of preparing International Standards is normally carried out through ISO technical
committees. Each member body interested in a subject for which a technical committee has been established has
the right to be represented on that committee. International organizations, governmental and non-governmental, in
liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical
Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this part of ISO 10414 may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 10414-1 was prepared by Technical Committee ISO/TC 67, Materials, equipment and
offshore structures for petroleum and natural gas industries, Subcommittee SC 3, Drilling and completion fluids,
and well cements.
ISO 10414 consists of the following parts, under the general title Petroleum and natural gas industries — Field
testing of drilling fluids:
� Part 1: Water-based fluids
� Part 2: Oil-based fluids
Annexes A to H of this part of ISO 10414 are for information only.
iv © ISO 2001 – All rights reserved

Introduction
This part of ISO 10414 is based on API RP 13B-1, second edition, September 1997 [2].
As with any laboratory procedure requiring the use of potentially hazardous chemicals, the user is expected to have
proper knowledge and received training in the use and disposal of these chemicals. The user is responsible for
compliance with all applicable local, regional and national requirements for worker and local health, safety and
environmental liability.
In this part of ISO 10414, where practical, U.S. customary units are included in brackets for information.
INTERNATIONAL STANDARD ISO 10414-1:2001(E)
Petroleum and natural gas industries — Field testing of drilling
fluids —
Part 1:
Water-based fluids
1 Scope
This part of ISO 10414 provides standard procedures for the determining following characteristics of water-based
drilling fluids:
a) drilling fluid density (mud weight);
b) viscosity and gel strength;
c) filtration;
d) water, oil and solids contents;
e) sand content;
f) methylene blue capacity;
g) pH;
h) alkalinity and lime content;
i) chloride content;
j) total hardness as calcium.
Annexes A, B, C and E provide additional test methods which may be used for
k) chemical analysis for calcium, magnesium, calcium sulfate, sulfide, carbonate, potassium;
l) determination of shear strength;
m) determination of resistivity;
n) drill pipe corrosion monitoring.
Annexes D, F, G and H provide procedures that may be used for
o) removal of air;
p) sampling, inspection and rejection;
q) rig-site sampling;
r) calibration and verification of glassware, thermometers, viscometers, retort kit cup and drilling fluid balances.
2 Term and definition
For the purposes of this part of ISO 10414, the following term and definition applies.
2.1
ACS reagent grade
chemical meeting the purity standards specified by the American Chemical Society (ACS)
3 Abbreviated terms
ACS American Chemical Society
AISI American Iron and Steel Institute
CAS Chemical Abstracts Service
EDTA ethylenediaminetetraacetic acid
HT/HP high temperature, high pressure
meq milliequivalents
OCMA Oilfield Chemical Manufacturer’s Association
PTFE polytetrafluoroethylene
QAS quaternary ammonium salt
STPB sodium tetraphenyl borate
TC to contain
TD to deliver
4 Drilling fluid density (mud weight)
4.1 Principle
This test procedure is a method for determining the mass of a given volume of liquid (= density). Drilling fluid
density is expressed as grams per cubic centimetre, or kilograms per cubic metre.
4.2 Apparatus
3 3
4.2.1 Any density-measuring instrument of accuracy to within 0,01 g/cm or 10 kg/m .
The mud balance is the instrument generally used for drilling-fluid density determinations. The mud balance is
designed such that the drilling-fluid holding cup, at one end of the beam, is balanced by a fixed counterweight at
the other end, with a sliding-weight rider free to move along a graduated scale. A level-bubble is mounted on the
beam to allow for accurate balancing. Attachments for extending the range of the balance may be used when
necessary.
The instrument should be calibrated frequently with fresh water. Fresh water should give a reading of 1,00 g/cm or
1 000 kg/m at 21�C(70�F). If it does not, adjust the balancing screw or the amount of lead shot in the well at the
end of the graduated arm as required.
2 © ISO 2001 – All rights reserved

4.2.2 Thermometer,witharangeof0�C to 105�C(32�Fto 220�F).
4.3 Procedure
4.3.1 The instrument base should be set on a flat, level surface.
4.3.2 Measure the temperature of the drilling fluid and record.
4.3.3 Fill the clean, dry cup with drilling fluid to be tested; put the cap on the filled drilling-fluid holding cup and
rotate the cap until it is firmly seated. Ensure that some of the drilling fluid is expelled through the hole in the cap in
order to free any trapped air or gas (see annex D for information on air or gas removal).
4.3.4 Holding the cap firmly on the drilling-fluid holding cup (with cap hole covered), wash or wipe the outside of
the cup clean and dry.
4.3.5 Place the beam on the base support and balance it by moving the rider along the graduated scale. Balance
is achieved when the bubble is under the centreline.
4.3.6 Read the drilling fluid density at the edge of the rider toward the drilling-fluid holding cup. Make appropriate
corrections when a range extender is used.
4.4 Calculation
3 3
4.4.1 Report the drilling fluid density to the nearest 0,01 g/cm or 10 kg/m .
4.4.2 To convert the reading to other units, use the following:
ρ =1000� g/cm (1)
ρ = 16� lb/ft (2)
ρ = 119,8� lb/USgal (3)
whereρ is the density, expressed in kilograms per cubic metre.
DFG = 9,81� g/cm (4)
DFG = 0,022 6� psi/1 000 ft (5)
where DFG is the drilling fluid gradient, expressed in kilopascals per metre.
A list of density conversions is given in Table 1.
Table 1 — Density conversion
Grams Kilograms Pounds Pounds per
per cubic per cubic per US cubic foot
a
centimetre metre gallon
3 3 3
g/cm kg/m (lb/US gal) (lb/ft )
0,70 700 5,8 43,6
0,80 800 6,7 49,8
0,90 900 7,5 56,1
b
1,00 1 000 8,345 62,3
1,10 1 100 9,2 68,5
1,20 1 200 10,0 74,8
1,30 1 300 10,9 81,0
1,40 1 400 11,7 87,2
1,50 1 500 12,5 93,5
1,60 1 600 13,4 99,7
1,70 1 700 14,2 105,9
1,80 1 800 15,0 112,1
1,90 1 900 15,9 118,4
2,00 2 000 16,7 124,6
2,10 2 100 17,5 130,8
2,20 2 200 18,4 137,1
2,30 2 300 19,2 143,3
2,40 2 400 20,0 149,5
2,50 2 500 20,9 155,8
2,60 2 600 21,7 162,0
2,70 2 700 22,5 168,2
2,80 2 800 23,4 174,4
2,90 2 900 24,2 180,7
a
Same value as relative density.
b
Accurate conversion factor.
5 Alternative drilling fluid density method
5.1 Principle
The density of a drilling fluid containing entrained air or gas can be determined more accurately by using the
pressurized mud balance. The pressurized mud balance is similar in operation to the conventional mud balance,
the difference being that the slurry sample can be placed in a fixed-volume sample cup under pressure.
4 © ISO 2001 – All rights reserved

The purpose of placing the sample under pressure is to minimize the effect of entrained air or gas upon slurry
density measurements. By pressurizing the sample cup, any entrained air or gas will be decreased to a negligible
volume, thus providing a slurry density measurement more closely in agreement with that which will be realized
under downhole conditions.
5.2 Apparatus
3 3
5.2.1 Any density-measuring instrument of accuracy to within 0,01 g/cm or 10 kg/m .
The pressurized mud balance is the instrument generally used for pressurized drilling-fluid density determinations.
The pressurized mud balance is designed such that the drilling-fluid holding cup and screw-on lid, at one end of the
beam, is balanced by a fixed counterweight at the other end, with a sliding-weight rider free to move along a
graduated scale. A level-bubble is mounted on the beam to allow for accurate balancing.
Calibrate the instrument frequently with fresh water. Fresh water should give a reading of 1,00 g/cm or
1 000 kg/m at 21�C(70�F). If it does not, adjust the balancing screw or the amount of lead shot in the well at the
end of the graduated arm as required.
5.2.2 Thermometer,witharangeof0�C to 105�C(32�Fto 220�F).
5.3 Procedure
5.3.1 Measure the temperature of the drilling fluid and record.
5.3.2 Fill the sample cup to a level slightly below the upper edge of the cup (approximately 6 mm).
5.3.3 Place the lid on the cup with the attached check-valve in the down (open) position. Push the lid downward
into the mouth of the cup until surface contact is made between the outer skirt of the lid and the upper edge of the
cup. Any excess slurry will be expelled through the check-valve. When the lid has been placed on the cup, pull the
check-valve up into the closed position, rinse off the cup and threads with water, and screw the threaded cap on
the cup.
5.3.4 The pressurizing plunger is similar in operation to a syringe. Fill the plunger by submersing its end in the
slurry with the piston rod completely inside. Then draw the piston rod upward, thereby filling the cylinder with slurry.
This volume should be expelled with the plunger action and refilled with fresh slurry sample to ensure that this
plunger volume is not diluted with liquid remaining from the last clean-up of the plunger mechanism.
5.3.5 Push the nose of the plunger onto the mating O-ring surface of the cap valve. Pressurize the sample cup
by maintaining a downward force on the cylinder housing in order to hold the check-valve down (open) and at the
same time to force the piston rod inside. A force of approximately 225 N (50 lbf) or greater should be maintained on
the piston rod.
5.3.6 The check-valve in the lid is pressure-actuated; when the inside of the cup is pressurized, the check-valve
is pushed upward into the closed position. To close the valve, gradually ease up on the cylinder housing while
maintaining pressure on the piston rod. When the check-valve closes, release pressure on the piston rod before
disconnecting the plunger.
5.3.7 The pressurized slurry sample is now ready for weighing. Rinse the exterior of the cup and wipe dry. Place
the instrument on the knife edge. Move the sliding weight to the right or left until the beam is balanced. The beam is
balanced when the attached bubble is centred between the two black marks. Read the density from one of the four
calibrated scales on the arrow side of the sliding weight. The density can be read directly in units of g/cm , lb/gal,
and lb/ft or as a drilling fluid gradient in psi/1 000 ft.
5.3.8 To release the pressure inside the cup, reconnect the empty plunger assembly and push downward on the
cylinder housing.
5.3.9 Clean the cup and rinse thoroughly with water. For best operation in water-based slurries, the valve should
be greased frequently with waterproof grease.
5.4 Calculation
3 3
Report the drilling fluid density to the nearest 0,01 g/cm or 10 kg/m .
For conversions, use the formula given in 4.5.2.
6 Viscosity and gel strength
6.1 Principle
Viscosity and gel strength are measurements that relate to the flow properties (rheology) of drilling fluids. The
following instruments are used to measure viscosity and/or gel strength of drilling fluids:
a) Marsh funnel — a simple device for indicating viscosity on a routine basis;
b) direct-indicating viscometer — a mechanical device for measurement of viscosity at varying shear rates.
NOTE Information on the rheology of drilling fluids may be found in [3].
6.2 Determination of viscosity using the Marsh funnel
6.2.1 Apparatus
6.2.1.1 Marsh funnel, calibrated to out-flow 946 ml (1 quart) of fresh water at a temperature of (21� 3)�C
[(70� 5)�F] in (26� 0,5) s, with a graduated cup as a receiver.
6.2.1.1.1 Funnel cone, of length 305 mm (12,0 in), diameter 152 mm (6,0 in) and a capacity to bottom of screen
of 1 500 ml (1,6 quarts).
6.2.1.1.2 Orifice, of length 50,8 mm (2,0 in) and inside diameter 4,7 mm (0,185 in).
6.2.1.1.3 Screen, with 1,6 mm (0,063 in) openings (12 mesh); fixed at 19,0 mm (0,748 in) below top of funnel.
6.2.1.2 Graduated cup, with capacity at least 946 ml (1 quart).
6.2.1.3 Stopwatch.
6.2.1.4 Thermometer,witharangeof0�C to 105�C(32�Fto 220�F).
6.2.2 Procedure
6.2.2.1 Cover the funnel orifice with a finger and pour freshly sampled drilling fluid through the screen into the
clean, upright funnel. Fill until fluid reaches the bottom of the screen.
6.2.2.2 Remove finger and start stopwatch. Measure the time for drilling fluid to fill to 946 ml (1 quart) mark of
the cup.
6.2.2.3 Measure temperature of the fluid, in degrees Celsius (degrees Fahrenheit).
6.2.2.4 Report the time (6.2.2.2), to the nearest second, as the Marsh funnel viscosity. Report the temperature
(6.2.2.3) of fluid to the nearest degree Celsius (degree Fahrenheit).
6 © ISO 2001 – All rights reserved

6.3 Determination of viscosity and/or gel strength using a direct-indicating viscometer
6.3.1 Apparatus
6.3.1.1 Direct-indicating viscometer
This type of viscometer is a rotational instrument powered by an electric motor or a hand crank. Drilling fluid is
contained in the annular space between two concentric cylinders. The outer cylinder or rotor sleeve is driven at a
constant rotational velocity. The rotation of the rotor sleeve in the fluid produces a torque on the inner cylinder or
bob. A torsion spring restrains the movement of the 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 300 r/min and 600 r/min.
A direct-indicating viscometer shall meet the following specifications:
a) Rotor sleeve
Inside diameter
36,83 mm (1,450 in)
Total length 87,0 mm (3,425 in)
Scribed line 58,4 mm (2,30 in) above the bottom of sleeve, with two rows of 3,18 mm (0,125 in) holes
spaced 120� (2,09 radians) apart, around rotor sleeve just below scribed line.
b) Bob, closed, with flat base and tapered top
Diameter
34,49 mm (1,358 in)
Cylinder length 38,0 mm (1,496 in)
c) Torsion spring constant
386 dyne-cm/degree deflection.
d) Rotor sleeve speed
High speed
600 r/min
Low speed 300 r/min
NOTE Other rotor speeds are available in viscometers from various manufacturers.
6.3.1.2 Stopwatch.
6.3.1.3 Suitable container, e.g. the cup provided with the viscometer.
6.3.1.4 Thermometer,witharangeof0 �Cto105�C(32�Fto220�F).
6.3.2 Procedure
6.3.2.1 Place the sample in a container and immerse the rotor sleeve exactly to the scribed line.
Measurements in the field should be made with minimum delay (within 5 min, if possible) and at a temperature as
near as practical to that of the drilling fluid at the place of sampling, but not differing by more than 6 °C(10 °F). The
place of sampling should be stated on the test report.
WARNING — Maximum recommended operating temperature is 90 ��C(200 ��F). If fluids have to be tested
�� ��
above this temperature, a solid metal bob or a hollow metal bob with a completely dry interior should be
used. Liquid trapped inside a hollow bob may vaporize when immersed in high temperature fluid and cause
the bob to explode.
6.3.2.2 Record the temperature of the sample.
6.3.2.3 With the sleeve rotating at 600 r/min, wait for viscometer dial reading to reach a steady value (the time
required is dependent on the drilling-fluid characteristics). Record the dial reading for 600 r/min.
6.3.2.4 Reduce the rotor speed to 300 r/min and wait for viscometer dial reading to reach a steady value.
Record the dial reading for 300 r/min.
6.3.2.5 Stir drilling fluid sample for 10 s at 600 r/min.
6.3.2.6 Allow drilling fluid sample to stand undisturbed for 10 s. Slowly and steadily turn the hand-wheel in the
appropriate direction to produce a positive dial reading. The maximum reading is the initial gel strength. For
instruments having a speed of 3 r/min, the maximum reading attained after starting rotation at 3 r/min is the initial
gel strength. Record the initial gel strength (10-second gel) in pascals (or in pounds per 100 square feet).
6.3.2.7 Restir the drilling fluid sample at 600 r/min for 10 s and then allow the drilling fluid to stand undisturbed
for 10 min. Repeat the measurements as in 6.3.2.6 and report the maximum reading as the 10-minute gel in
pascals (or in pounds per 100 square feet).
6.3.3 Calculation
� = R – R (6)
P 600 300
YP = 0,48 � (R –� ) (7)
P
� = R / 2 (8)
A
where
� is the plastic viscosity, in millipascal seconds;
P
NOTE Plastic viscosity is commonly known in the industry by the abbreviation PV.
YP is the yield point, in pascals;
� is the apparent viscosity, in millipascal seconds;
A
R is the dial reading at 600 r/min, in pascals (or in lb/100 ft );
R is the dial reading at 300 r/min, in pascals (or in lb/100 ft ).
NOTE 1 1 cP = 1 mPa�s
NOTE 2 When calculating values in U.S. customary units, the yield point (in lb/100 ft )iscalculatedasfollows:
YP = R –�
300 P
7 Filtration
7.1 Principle
Measurement of the filtration behaviour and filter cake-building characteristics of a drilling fluid are fundamental to
drilling-fluid control and treatment, as are the characteristics of the filtrate such as oil, water or emulsion content.
These characteristics are affected by the types and quantities of solids in the fluid and their physical and chemical
interactions which, in turn, are affected by temperature and pressure. Therefore, tests are run at both low
pressure/low temperature and high pressure/high temperature, and each requires different equipment and
techniques.
8 © ISO 2001 – All rights reserved

7.2 Low temperature/low pressure test
7.2.1 Apparatus
7.2.1.1 Filter press, consisting mainly of a cylindrical drilling-fluid cell having an inside diameter of 76,2 mm
(3 in) and a height of at least 64,0 mm (2,5 in).
This cell is made of materials resistant to strongly alkaline solutions, and is so fitted that a pressure medium can be
conveniently admitted into, and bled from the top. It shall also be fitted such that a sheet of 90 mm (3,54 in)
diameter filter paper can be placed in the bottom of the cell just above a suitable support. The filtration area is
2 2
(45,8� 0,6) cm [(7,1� 0,1) in ]. Below the support is a drain tube for discharging the filtrate into a graduated
cylinder. Sealing is accomplished with gaskets, and the entire assembly supported by a stand. Pressure can be
applied with any non-hazardous fluid medium. Presses are equipped with pressure regulators and can be obtained
with portable pressure cylinders, midget pressure cartridges or means for utilizing hydraulic pressure. To obtain
1)
correlative results, one thickness of the proper 90 mm diameter filter paper (e.g. Whatman No. 50, S&S No. 576
or equivalent) shall be used.
2 2
The low temperature/low pressure filter press should have a filter area of 45,2 cm to 46,4 cm , which corresponds
to a diameter of 75,86 mm to 76,86 mm (2,987 in to 3,026 in). The filter press gasket is the determining factor of
the filter area. It is recommended that a filter press gasket used be tested by a conical gauge that has the
maximum (76,86 mm) and the minimum (75,86 mm) diameters marked on it. Any filter press gasket found out of
these ranges (either larger or smaller than the markings) shall be discarded.
NOTE Results obtained from the use of a filter press with different filter area do not directly correlate with the results
obtained when using the standard-sized press.
7.2.1.2 Timer, with at least a 30 min interval.
7.2.1.3 Graduated cylinder (TC), of volume 10 ml or 25 ml.
7.2.2 Procedure
7.2.2.1 Be sure each part of the cell, particularly the screen, is clean and dry, and that the gaskets are not
distorted or worn. Pour the drilling fluid sample into the cell to within 1 cm to 1,5 cm (0, 4 in to 0,6 in) of the top (to
minimize CO contamination of filtrate), and complete the assembly with the filter paper in place.
7.2.2.2 Place a dry graduated cylinder under the drain tube to collect the filtrate. Close the relief valve and
adjust the regulator so that a pressure of 690 kPa� 35 kPa (100 psi� 5 psi) is applied within 30 s or less. The test
period begins at the time of pressure application.
7.2.2.3 At the end of 30 min, measure the volume of filtrate collected. Shut off the flow through the pressure
regulator and open the relief valve carefully. The time interval, if other than 30 min, shall be reported.
7.2.2.4 Report the volume of filtrate in millilitres (to the nearest 0,1 ml) and the initial drilling fluid temperature
in degrees Celsius (degrees Fahrenheit). Save the filtrate for chemical analysis.
7.2.2.5 Remove the cell from the frame, first making certain that all pressure has been relieved. Carefully save
the filter paper with a minimum of disturbance to the cake, disassemble the cell and discard the drilling fluid. Wash
the filter cake on the paper with a gentle stream of water.
7.2.2.6 Measure and report the thickness of the filter cake, to the nearest millimetre.
7.2.2.7 Although cake descriptions are subjective, such notations as hard, soft, tough, rubbery, firm, etc., may
convey important information of cake quality.
1) Whatman No. 50 and S&S No. 576 are examples of suitable products available commercially. This information is given for
the convenience of users of this part of ISO 10414 and does not constitute an endorsement by ISO of these products.
7.3 High temperature/high pressure (HT/HP) test
7.3.1 Apparatus
7.3.1.1 HT/HP filter press, consisting of a controlled pressure source (CO or nitrogen), regulators, a drilling-
fluid cell able to contain working pressures from 4 000 kPa to 8 900 kPa (600 psi to 1 300 psi), a system for heating
the cell, a pressurized collection cell able to maintain proper back-pressure (see Table 2) in order to prevent
flashing or evaporation of the filtrate, and a suitable stand. The drilling-fluid cell has a thermometer well, oil-
resistant gaskets, a support for the filter medium and a valve on the filtrate delivery tube to control flow from the
cell. It may be necessary to replace the gaskets frequently.
WARNING — Rigid adherence to manufacturers' recommendations as to sample volumes, equipment
temperatures and pressures is essential. Failure to do so could result in serious injury.
Do not use nitrous oxide cartridges as pressure sources for HT/HP filtration. Under temperature and
pressure, nitrous oxide can detonate in the presence of grease, oil or carbonaceous materials. Nitrous
oxide cartridges shall be used only for Garrett gas train carbonate analysis.
2)
7.3.1.2 Filter medium .
a) Filter paper, Whatman No. 50 or equivalent, for temperatures to 200�C(400�F).
b) Porous disc, Dynalloy X-5 or equivalent, for temperatures above 200 �C (400 �F). A new discisrequired for
each test.
7.3.1.3 Timer, with at least a 30 min interval.
7.3.1.4 Thermometer, with arangeupto 260�C (500�F).
7.3.1.5 Graduated cylinder (TC), with a volume of 25 ml or 50 ml.
7.3.1.6 High-speed mixer.
7.3.2 Procedure for temperatures to 150 ����C (300 ����F)
7.3.2.1 Place the thermometer in the well in the jacket and preheat to 6�C(10�F) above the desired
temperature. Adjust the thermostat to maintain the desired temperature.
7.3.2.2 Stir drilling fluid sample for 10 min with a high speed mixer. Close the bottom valve and pour the
drilling fluid sample into the drilling fluid cell, being careful not to fill closer than 1,5 cm (0,6 in) from the top to allow
for expansion. Install the filter paper.
7.3.2.3 Complete the assembly of the cell and, with both top and bottom valves closed, place it in the heating
jacket. Transfer the thermometer to the well in the drilling fluid cell.
7.3.2.4 Connect the high-pressure collection cell to the bottom valve and lock in place.
7.3.2.5 Connect a regulated pressure source to the top valve and collection cell, and lock in place.
7.3.2.6 Keeping the valves closed, adjust top and bottom regulators to 690 kPa (100 psi). Open the top valve,
applying 690 kPa (100 psi) to the drilling fluid. Maintain this pressure until the desired temperature is stabilized. The
sample in the filter cell should never be heated for a period exceeding a total of 1 h.
2) Whatman No. 50 and Dynalloy X-5 discs are examples of suitable products available commercially. Dynalloy is a trade
name of a product supplied by Memtec America Corporation. This information is given for the convenience of users of this part
of ISO 10414 and does not constitute an endorsement by ISO of these products.
10 © ISO 2001 – All rights reserved

7.3.2.7 When the sample reaches the selected test temperature, increase the pressure of the top pressure unit
to 4 140 kPa (600 psi) and open the bottom valve to start filtration. Collect the filtrate for 30 min, maintaining the
selected temperature within � 3�C(� 5�F). If back-pressure rises above 690 kPa (100 psi) during the test,
cautiously reduce the pressure by drawing off a portion of the filtrate. Record the total volume collected, the
temperature, pressure and time.
2 2
7.3.2.8 Correct thefiltrate volumetoafilter area of 45,8cm (7,1 in ). For example, if the filter area is
2 2
22,6 cm (3,5 in ), double the filtrate volume reported.
7.3.2.9 At the end of test, close top and bottom valves on the drilling fluid cell. Bleed pressure from the
regulators.
WARNING — Pressure in the drilling fluid cell will still be approximately 4 140 kPa (600 psi). To avoid
possible serious injury, keep cell upright and cool to room temperature, then bleed pressure from cell
before disassembling.
7.3.2.10 Remove the cell from the heating jacket, first making certain that the bottom and top valves are tightly
shut and all pressure is off regulators. Using extreme care to save the filter paper, place the cell upright, open the
valve to bleed pressure from cell contents and open. Discard drilling fluid, and retrieve filter cake. Wash filter cake
on the paper with a gentle stream of water.
7.3.2.11 Measure and report the thickness of the filter cake, to the nearest millimetre.
7.3.2.12 Although cake descriptions are subjective, such notations as hard, soft, tough, rubbery, firm, etc., may
convey important information of cake quality.
7.3.3 Procedure for temperatures above 150 ��C (300 ��F)
�� ��
7.3.3.1 Place the thermometer in the well in the jacket and preheat to 6�C(10�F) above the desired
temperature. Adjust the thermostat to maintain the correct temperature.
7.3.3.2 Stir drilling fluid sample for 10 min with a high speed mixer. Close the bottom valve and pour the
drilling fluid sample into the drilling fluid cell, being careful not to fill the cell closer than 4 cm (1,5 in) from the top to
allow for expansion. Install the proper filter medium (see 7.3.1.2).
CAUTION — Not all manufacturers' equipment can be used above 150 ����C(300 ����F). Failure to know the
pressure/temperature rating of equipment in use could result in serious injury. Testing at high temperature
and high pressure calls for added safety precautions.
All pressure cells should be equipped with manual relief valves. Heating jackets should be equipped with both an
overheat safety fuse and thermostatic cut-off. Vapour pressure of the liquid phase of drilling fluids becomes an
increasingly critical design factor as test temperatures are raised. Water vapour pressures at various temperatures
are shown in Table 2.
7.3.3.3 Complete the assembly of the cell, and with top and bottom valves closed, place the drilling fluid cell in
the heating jacket. Transfer the thermometer to the well in the drilling fluid cell.
7.3.3.4 Connect the high-pressure collection cell to the bottom valve, and lock in place.
7.3.3.5 Connect the regulated pressure source to the top valve and the collection cell, and lock in place.
7.3.3.6 With top and bottom valves closed, apply the recommended back-pressure (see Table 2) for the test
temperature to both top and bottom. Open the top valve, applying the same pressure to the drilling fluid while
heating. Maintain this pressure until the test temperature is reached and stabilized.
7.3.3.7 When the temperature of the sample reaches the test temperature, increase the pressure on the top by
3 450 kPa (500 psi) over the back-pressure being held, and open the bottom valve to begin filtration. Collect the
filtrate for 30 min, holding the test temperature within � 3�C(� 5�F) and maintaining the proper back-pressure. If
the back-pressure should begin to rise, it can be reduced by cautiously drawing off a small portion of the filtrate.
The sample in the filter cell should never be heated for a period exceeding a total of 1 h.
7.3.3.8 After the test period, close both top and bottom valves on the pressure cell and bleed pressure from
the regulators. Allow a minimum of 5 min for the filtrate to cool to avoid vaporizing, then cautiously drain and record
the total volume. Also record the temperature, pressures and time. Be sure to allow sufficient time for all the filtrate
to drain from the receiver.
WARNING — Pressure inside the filter cell could be as high as 6 500 kPa (950 psi). To avoid possible
serious injury, keep cell upright and cool to room temperature, then bleed pressure from cell before
disassembly.
2 2
7.3.3.9 Correct thefiltrate volumetoafilter area of 45,8cm (7,1 in ). For example, if the filter area is
2 2
22,6 cm (3,5 in ), double the filtrate volume reported.
7.3.3.10 Remove the cell from the heating jacket, first making certain that the bottom and top valves are tightly
shut and all pressure is off regulators. Using extreme care to save the filter paper, place the cell upright, open the
valve to bleed pressure from cell contents and open. Discard drilling fluid, and retrieve filter cake. Wash filter cake
on the paper with a gentle stream of water.
7.3.3.11 Measure and report the thickness of the filter cake, to the nearest millimetre.
7.3.3.12 Although cake descriptions are subjective, such notations as hard, soft, tough, rubbery, firm, etc., may
convey important information of cake quality.
Table 2 — Recommended minimum back-pressure
Test temperature Vapour pressure Minimum back
pressure
°C °F kPa psi kPa psi
100 212 101 14,7 690 100
120 250 207 30 690 100
150 300 462 67 690 100
Limit of "normal" field testing
175 350 932 135 1 104 160
200 400 1 704 247 1 898 275
230 450 2 912 422 3 105 450
8 Water, oil and solids contents
8.1 Principle
The retort instrument provides a means for separating and measuring the volumes of water, oil and solids
contained in a sample of water-based drilling fluid. In the retort, a known volume of a whole drilling-fluid sample is
heated to vaporize the liquid components, which are then condensed and collected in a graduated receiver. Liquid
volumes are determined directly from reading the oil and water phases in the receiver. The total volume of solids
(suspended and dissolved) is obtained by difference (total sample volume minus liquid volume). Calculations are
necessary to determine the volume of suspended solids, since any dissolved solids will be retained in the retort.
The relative volumes of low gravity solids and weighting material can also be calculated. Knowledge of the solids
concentration and composition is considered basic to viscosity and filtration control in water-based drilling fluids.
12 © ISO 2001 – All rights reserved

8.2 Apparatus
8.2.1 Retort instrument.
Retorts of two sizes (10 ml and 20 ml) are commonly available. Specifications for these retorts are given below.
8.2.1.1 Sample cup.
Standard cup sizes are 10 ml (precision� 0,05 ml) and 20 ml (precision� 0,10 ml).
NOTE Other sample cup sizes are available from manufacturers of this equipment.
8.2.1.2 Liquid condenser, of sufficient mass to cool the oil and water vapours below their vaporization
temperature prior to leaving the condenser.
8.2.1.3 Heating element, of sufficient wattage to raise the temperature of the sample above the vaporization
point of the liquid components within 15 min without causing solids boil-over.
8.2.1.4 Temperature control (optional), capable of limiting the temperature of the retort to 500�C� 40�C
(930�F� 70 �F).
8.2.2 Liquid receiver (TC), specially designed cylindrical glassware with a rounded bottom to facilitate cleaning
and a funnel-shaped top to catch falling drops, meeting the following specifications:
Total volume: 10 ml 20 ml 50 ml
Precision(0to100%): � 0,05 ml � 0,05 ml � 0,05 ml
Frequency of graduation marks (0 to 100 %): 0,10 ml 0,10 ml 0,10 ml
Calibration: To contain “TC” at 20 °C(68 °F)
Scale: ml, cm or volume fraction (as percent)
Material: Transparent, and inert to oil, water and salt solutions at temperatures up to 32 °C(90 °F).
The receiver volume should be verified gravimetrically. The procedure and calculations are provided in annex H.
8.2.3 Fine steel wool, oil-free.
“Liquid steel wool” or similar products should not be used for this application.
8.2.4 High-temperature silicone grease, to be used as a thread seal and a lubricant.
8.2.5 Pipe cleaners.
8.2.6 Putty knife or spatula, with blade shaped to fit the inside dimensions of the sample cup of the retort.
8.2.7 Marsh funnel.
8.2.8 Defoaming agent.
8.2.9 Corkscrew.
8.3 Procedure
8.3.1 Be sure that the retort sample cup, condenser passage and liquid receiver are clean, dry and cooled from
previous use. The inside of the sample cup and lid shall be thoroughly cleaned with a putty knife or spatula prior to
each test. Periodically, the interior of the sample cup should also be lightly polished with steel wool. The condenser
passage should also be cleaned and dried before each test using pipe cleaners. A build-up of material in the
condenser can decrease condensation efficiency and cause erroneous liquid readings in a test.
NOTE Procedure will vary slightly depending on type of retort used. See manufacturers' instructions for complete
procedure.
8.3.2 Collect a representative sample of water-based drilling fluid and allow it to cool to approximately 26�C
(80�F). Screen the sample through the 1,68 mm (0,066 in) (12 mesh) screen on the Marsh funnel to remove lost
circulation material, large cuttings or debris.
8.3.3 If drilling fluid sample contains gas or air, add two to three drops of defoaming agent to about 300 ml of
drilling fluid and stir slowly for 2 min to 3 min to release gases.
8.3.4 Lubricate the threads on the sample cup and condenser tube with a light coating of silicone grease. This
prevents vapour loss through the threads and also facilitates disassembly of the equipment and cleaning at the end
of the test.
8.3.5 Lightly pack a ring of steel wool into the chamber above the sample cup. Use only enough steel wool to
prevent boil-over of solids into the liquid receiver.
NOTE This is determined from experience.
8.3.6 Fill the retort sample cup with degassed water-based drilling fluid, see 8.3.3. See annex D for information
onairorgas removal.
8.3.7 Carefully place the lid on the sample cup and allow an overflow of the sample through the hole in the lid to
ensure that the correct volume of sample is in the cup.
8.3.8 With the lid held tightly in place, wipe the overflow from the sample cup and lid. Be sure that the sample
cup threads are still covered with silicone grease after wiping, and that the hole in the lid is not plugged.
8.3.9 Screw the retort cup onto the retort chamber with its condenser.
8.3.10 Place a clean, dry, liquid receiver under the condenser discharge tube.
8.3.11 Heat the retort and observe the liquid falling from the condenser. Continue heating for 10 min after the last
condensate is collected.
8.3.12 Remove the liquid receiver from the retort. Note whether solids are in the liquid which was recovered. If so,
the whole drilling fluid has boiled over from the sample cup and the test shall be repeated from 8.3.6.
8.3.13 Read the volumes of water and oil in the liquid receiver after it has cooled to ambient temperature. Record
the volumes (or volume percentages) of water and oil collected.
8.3.14 Cool the retort, remove the steel with corkscrew and clean the sample cup with a putty knife or spatula.
8.4 Calculation
8.4.1 Using the measured volumes of oil and water and the volume of the original whole drilling fluid sample
(10 ml or 20 ml), calculate as percentages the volume fractions of water, oil and total solids in the drilling fluid.
a) Volume fraction water:
V
wa
V��100 (9)
w
V
sa
where
V is the volume fraction of water, expressed as a percentage of the total sample volume;
w
V is the volume of water, in millilitres;
wa
V is the volume of the drilling fluid sample, in millilitres.
sa
14 © ISO 2001 – All rights reserved

b) Volume fraction oil:
V
oa
V��100 (10)
o
V
sa
where
V is the volume fraction of oil, expressed as a percentage of the total sample volume;
o
V is the volume of oil, in millilitres;
oa
V is the volume of
...