SIST EN ISO 13503-1:2005

SLOVENSKI STANDARD
SIST EN ISO 13503-1:2005
01-junij-2005
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Petroleum and natural gas industries - Completion fluids and materials - Part 1:
Measurement of viscous properties of completion fluids (ISO 13503-1:2003)
Erdöl- und Erdgasindustrie - Komplettierungsflüssigkeiten und Materialien - Teil 1:
Messung der Fließeigenschaften von Komplettierungsflüssigkeiten (ISO 13503-1:2003)
Industries du pétrole et du gaz naturel - Fluides de complétion et matériaux - Partie 1:
Mesures des propriétés visqueuses des fluides de complétion (ISO 13503-1:2003)
Ta slovenski standard je istoveten z: EN ISO 13503-1:2005
ICS:
75.180.30 Oprema za merjenje Volumetric equipment and
prostornine in merjenje measurements
SIST EN ISO 13503-1:2005 en,fr
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 13503-1:2005

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SIST EN ISO 13503-1:2005
EUROPEAN STANDARD
EN ISO 13503-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
March 2005
ICS 75.100
English version
Petroleum and natural gas industries - Completion fluids and
materials - Part 1: Measurement of viscous properties of
completion fluids (ISO 13503-1:2003)
Industries du pétrole et du gaz naturel - Fluides de Erdöl- und Erdgasindustrie - Komplettierungsflüssigkeiten
complétion et matériaux - Partie 1: Mesures des propriétés und Materialien - Teil 1: Messung der Fließeigenschaften
visqueuses des fluides de complétion (ISO 13503-1:2003) von Komplettierungsflüssigkeiten (ISO 13503-1:2003)
This European Standard was approved by CEN on 7 February 2005.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the Central Secretariat or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13503-1:2005: E
worldwide for CEN national Members.

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SIST EN ISO 13503-1:2005
EN ISO 13503-1:2005 (E)






Foreword



The text of ISO 13503-1:2003 has been prepared by Technical Committee ISO/TC 67
"Materials, equipment and offshore structures for petroleum and natural gas industries" of the
International Organization for Standardization (ISO) and has been taken over as EN ISO 13503-
1:2005 by Technical Committee CEN/TC 12 "Materials, equipment and offshore structures for
petroleum, petrochemical and natural gas industries" the secretariat of which is held by AFNOR.

This European Standard shall be given the status of a national standard, either by publication of
an identical text or by endorsement, at the latest by September 2005, and conflicting national
standards shall be withdrawn at the latest by September 2005.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.


Endorsement notice

The text of ISO 13503-1:2003 has been approved by CEN as EN ISO 13503-1:2005 without any
modifications.

2

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SIST EN ISO 13503-1:2005


INTERNATIONAL ISO
STANDARD 13503-1
First edition
2003-09-01

Petroleum and natural gas industries —
Completion fluids and materials —
Part 1:
Measurement of viscous properties of
completion fluids
Industries du pétrole et du gaz naturel — Fluides de complétion et
matériaux —
Partie 1: Mesures des propriétés visqueuses des fluides de complétion




Reference number
ISO 13503-1:2003(E)
©
ISO 2003

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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)
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©  ISO 2003
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ii © ISO 2003 — All rights reserved

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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope. 1
2 Terms and definitions. 1
3 Abbreviated terms. 2
4 Measurement and precision. 2
5 Fluid preparation. 2
6 Fluid preparation using shear-history simulation (optional). 3
6.1 General. 3
6.2 Requirements for proper shear-history simulation. 3
6.3 Conditions for sample delivery . 3
6.4 Conditions for standard shear-history simulation . 3
6.5 Operational considerations. 4
7 Instrument calibration . 5
8 Measurement procedures . 5
8.1 General. 5
8.2 Non-crosslinked fluids (see 2.6). 5
8.3 Viscoelastic fluids. 10
9 Calculation procedures . 11
9.1 General concepts . 11
9.2 Brief review of geometry-independent rheology vs. nominal rheology. 12
9.3 Limitations/problems that may produce erroneous results. 13
9.4 Calculation method for concentric-cylinder viscometers . 13
9.5 Bingham plastic parameters for completion fluids . 16
9.6 Calculations for optional shear-history simulation. 16
10 Test report. 17
Bibliography . 20

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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)
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 2.
The main task of technical committees is to prepare International Standards. 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 document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 13503-1 was prepared by Technical Committee ISO/TC 67, Materials, equipment and offshore structures
for petroleum, petrochemical and natural gas industries, Subcommittee SC 3, Drilling and completion fluids,
and well cements.
ISO 13503 consists of the following parts, under the general title Petroleum and natural gas industries —
Completion fluids and materials:
 Part 1: Measurement of viscous properties of completion fluids
The following part is under preparation:
 Part 2: Measurement of properties of proppants used in hydraulic fracturing and gravel-packing
operations
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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)
Introduction
For the purpose of this part of ISO 13503, completion fluids are defined as viscosified treating fluids used
during the completion or workover of a petroleum- or natural gas-producing well. The objective of this part of
ISO 13503 is to provide a standard procedure for measuring the viscous properties of single-phase, non-
particulate-laden completion fluids. These fluids are viscosified brines, gravel-pack carrier fluids, and
fracturing fluids. These fluids can be either crosslinked or non-crosslinked (aqueous, hydrocarbon- or acid-
based).
An optional shear-history simulation procedure is provided for fluids that are potentially shear-sensitive. This
procedure is designed to simulate the shearing effects experienced by a fluid in surface apparatus and during
the time it is being conveyed down the welbore. Shear-history simulation is most often used during the
development of new fracturing fluids to characterize their sensitivity to shear.
These standard procedures were compiled on the basis of several years of comparative testing, debate,
discussion, and continued research by the industry.
This standard procedure is largely based on API RP 39, third edition, May 1998 [1].
In this part of ISO 13503, where practical, U.S. Customary units are included in parentheses for convenience.

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SIST EN ISO 13503-1:2005

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SIST EN ISO 13503-1:2005
INTERNATIONAL STANDARD ISO 13503-1:2003(E)

Petroleum and natural gas industries — Completion fluids and
materials —
Part 1:
Measurement of viscous properties of completion fluids
1 Scope
This part of ISO 13503 provides consistent methodology for determining the viscosity of completion fluids
used in the petroleum and natural gas industries. For certain cases, methods are also provided to determine
the rheological properties of a fluid.
2 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
2.1
bob
fixed inner cylinder of a concentric-cylinder viscometer
2.2
completion fluid
any fluid used during the completion phase of a well
2.3
concentric-cylinder viscometer
rotational viscometer that consists of a concentric-cylindrical bob and a cylindrical rotor
2.4
elasticity
capability of a material to regain its original shape and condition upon removal of an acting stress
2.5
laminar flow
flow property of fluids in which all layers of the fluid move parallel to each other and no material is transferred
between layers
2.6
non-crosslinked fluid
linear, polymer-viscosified solution or any fluid that does not exhibit significant elasticity leading to the
Weissenberg effect (“bob climbing”)
2.7
rheology
science of the deformation and flow of matter
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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)
2.8
shear history
sequence of shear rates and temperatures applied to fluids prior to and during measurements
2.9
shear-history simulator
apparatus used to simulate shear history in a fluid
2.10
shear rate
rate at which one particle of fluid is sliding by another particle divided by the distance between those particles
2.11
shear stress
force required to sustain fluid flow
2.12
viscoelastic fluid
crosslinked polymer solution or other fluid that exhibits significant elasticity, leading to the Weissenberg effect
(bob climbing)
2.13
viscosity
measure of the internal friction of a fluid when caused to flow by an external force
3 Abbreviated terms
r/min revolutions per minute
pH negative logarithm (to the base 10) of hydrogen ion concentration
ASTM American Society for Testing Materials
DIN Deutsches Institut für Normung
4 Measurement and precision
Temperatures shall be measured to an accuracy of ± 1 °C (± 2 °F); pH shall be measured to an accuracy of
± 0,1 units. All other quantitative measurements shall be made to an accuracy of ± 2 %, unless specified
otherwise.
5 Fluid preparation
Certain aspects of sample preparation and handling can affect the viscosity or rheological properties of a fluid.
During all procedures, steps shall be taken to minimize entraining air into the fluid. Following preparation, all
fluids, except those intended to be used as fracturing fluids, shall be filtered through a filter of pore diameter
2 µm. Minimize the entrainment of air during the filtration process.
The procedure used to prepare the fluid sample shall be documented including the following information:
a) description and/or composition of the base fluid. Preparation of the fluid shall be described, starting with
the fluid source, such as deionized water, tap water, seawater (location), or type of oil;
b) identification of mixing apparatus, container volume, and total volume of fluid prepared;
c) identification of each fluid component and amount added;
d) the order and method of addition of each component;
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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)
e) mixing speeds, with time at each speed;
f) ageing or holding time prior to measurements, if required;
g) temperature (required only for fracturing fluids);
h) pH (for aqueous fluids, where applicable);
i) all other aspects of the fluid preparation which are known to affect the outcome of the viscosity
measurement should be reported.
6 Fluid preparation using shear-history simulation (optional)
6.1 General
A shear-history simulation procedure is provided to simulate the effects of shear rate and time while a fluid is
being conveyed down well tubulars. This procedure is intended to characterize the effect of shear history on
fluid properties as part of the concept and development phase for a new fluid.
A shear-history apparatus is used to condition the fluid at specified shear rates, times and temperatures prior
to injection into a viscometer. It consists of mixing apparatus, pumping apparatus and tubing to simulate
significant aspects of the surface apparatus followed by shear conditions in the well tubulars. A shear-history
apparatus that satisfies the requirements can be generically classified as a tube or pipe flow device that
operates in the laminar flow regime. Flow shall occur in a single-pass mode.
A schematic diagram of a shear-history simulator connected to a pressurized concentric-cylinder viscometer is
shown in Figure 1. In laminar flow, the energy dissipation rate is the same in any shear-history apparatus even
if different tubing sizes are used. Thus the design and functioning of the apparatus can vary and still meet the
desired preconditioning criteria.
6.2 Requirements for proper shear-history simulation
The following procedures shall be followed:
a) record and report the test temperature;
b) ensure thorough mixing of all fluid-activating additive(s) immediately before the fluid enters the
shear-history tubing.
6.3 Conditions for sample delivery
The following conditions shall be fulfilled:
a) continuous delivery of base fluid while additives are added and cup is being filled;
b) constant shear rate within the shear-history tubing;
c) while fluid is being injected into the viscometer, shear rate within gap of the viscometer is a nominal
−1
100 s .
6.4 Conditions for standard shear-history simulation
The following conditions shall be fulfilled:
−1
a) for fluid temperatures less than or equal to 93 °C (200 °F), shear rate 675 s for 2,5 min;
−1
b) for fluid temperatures greater than 93 °C (200 °F), shear rate 1 350 s for 5 min.
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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)

Key
1 tubing coil
2 differential pressure measurement device (optional)
3 static mixing device
4 high-pressure syringe pump for final additive e.g. crosslinker or activator
5 high-pressure syringe pump for second additive, if needed
6 base (e.g. uncrosslinked) fluid in floating-piston accumulator
7 oil from pump moving floating piston, which in turn moves base fluid
8 positive displacement pump
9 reservoir for pump oil
10 flow diversion valve
11 container for fluid
12 pressurized concentric-cylinder viscometer
Figure 1 — Shear-history diagram
6.5 Operational considerations
The following conditions shall be fulfilled:
a) the pulsation caused by certain types of positive displacement pumps shall be minimized;
b) the base fluid shall be prepared, characterized and reported as described in Clause 5;
c) it is critical that a representative sample of the test fluid be injected into the viscometer; therefore initially
divert the fluid exiting the shear-history simulator away from the viscometer until stabilized flow and
composition are established;
d) unions, valves and similar fittings shall have internal diameters such that the shear rate of the fluid flowing
through them is essentially the same as within the tubing;
e) where the tubing is coiled, the diameter of the coil shall be larger than a critical value (see 9.6.2).
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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)
7 Instrument calibration
The instruments associated with these procedures shall be calibrated according to each manufacturer's
recommended method.
8 Measurement procedures
8.1 General
The procedures given in this clause are organized based on the type of fluid on which the measurement is
carried out. Where data are reported as being obtained using a particular procedure, the procedure given shall
be followed exactly. The fluid shall not react with instrument surfaces to generate contaminants, change
critical measurement dimensions, or impair proper mechanical operation.
8.2 Non-crosslinked fluids (see 2.6)
8.2.1 Introduction
For proper rheological characterization of this type of fluid, the fluid shall wet the walls of the measuring
chamber and remain within the annular gap.
8.2.2 Apparatus
For proper viscometric and rheological characterization, the apparatus used shall meet the following criteria:
a) the flow regime in the annular gap is laminar;
b) slippage of the fluid at the walls within the gap is negligible;
c) the fluid exhibits essentially time-independent behaviour during any given measurement.
1)
8.2.2.1 Non-pressurized concentric-cylinder viscometer , to measure viscous and rheological properties
at ambient pressure and at temperatures below the boiling point of the fluid.
Multiple-point measurements may be suitable for the calculation of rheological parameters.
Any non-pressurized concentric-cylinder viscometer that is described by the following dimensions may be
used (see Figure 2):
a) rotor (or sleeve)
1) inside diameter: 36,83 mm (1,450 in),
2) should be concentric with bob and extend the full length of bob;
b) bob
1) diameter: 34,49 mm (1,358 in),
2) cylinder length: 38 mm (1,496 in),
3) cylindrical body with a flat, closed bottom and a tapered top with a truncated cone angle of
60° degrees.


1) Examples of non-pressurized concentric-cylinder viscometers are the Fann Model 35 viscometer equipped with rotor 1,
bob 1 (R1B1) and appropriate spring; Chandler Model 3500 equipped with rotor 1 bob 1 (R1B1) and appropriate spring;
OFI Model 800 equipped with rotor 1 bob 1 (R1B1) and appropriate spring; or viscometers with equivalent geometry. This
information is given for the convenience of users of this part of ISO 13503 and does not constitute an endorsement by ISO
of these products.
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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)
Dimensions in millimetres

Key
1 torsion spring
2 rotor
3 bob
4 sample cup
5 stage
Figure 2 — Geometry of a non-pressurized concentric-cylinder viscometer
8.2.2.1.1 Calibration
Calibration shall be carried out according to the manufacturer's recommended procedure, or using a
standardized Newtonian calibration fluid traceable to an international/national standard such as ISO, ASTM,
DIN, or equivalent.
Calibration oil viscosity shall be selected to encompass the shear rate and shear stress envelopes to be
evaluated.
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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)
8.2.2.1.2 Operation
8.2.2.1.2.1 Preparation
Rotor and bob shall be properly aligned. All parts in contact with the fluid shall be at the same temperature as
the fluid. Use of the standard cup provided by the manufacturer is recommended. Other vessels may be used,
however the vertical space between the bottom of the bob and bottom of the vessel shall be at least 13 mm
(0,50 in).
8.2.2.1.2.2 Procedure
The non-crosslinked fluid sample to be tested shall be representative of the fluid as a whole, and air
entrainment shall be minimal. After being placed in the viscometer, the fluid is stirred for 10 s to 15 s at the
highest shear rate for which a measurement is to be made. Viscosity measurements should be made from
lowest to the highest shear rate. Record the average reading 20 s after reading is stabilized at each shear rate.
8.2.2.1.3 Calculations
In order to convert a reading in revolutions per minute to shear rate, use the following formula:
−1
1 r/min = 1,704 s
Viscometric calculations shall be performed according to the manufacturer's specified procedure.
For rheological calculations, see Clause 9.
2)
8.2.2.2 Pressurized concentric-cylinder viscometer , to measure the viscous and rheological properties
of completion fluids at elevated temperatures.
Pressurization minimizes the effect of entrained air on measured parameters and allows measurements to be
made at temperatures above the atmospheric boiling point of the sample. Multiple-point measurements may
be suitable for determining the rheological parameters of fluids.
Any pressurized concentric-cylinder viscometer with the dimensions shown in Figure 3 may be used.
8.2.2.2.1 Calibration
Measure the temperature of the fluid being tested according to the manufacturer's specified procedure which
shall be traceable to a national/international standard such as ISO, ASTM, DIN, or equivalent.
Measure the rotor or sleeve speed according to the manufacturer's specified tachometer calibration procedure
which shall be traceable to a national/international standard such as ISO, ASTM, DIN, or equivalent.
Use one of the following calibration methods:
a) preferred method
Verify system using a standardized Newtonian calibration fluid traceable to a national/international
standard such as ISO, ASTM, DIN or equivalent. A calibration oil viscosity shall be selected to
encompass the shear rate/shear stress envelope to be evaluated. The calibration shall be conducted at
ambient pressure.
NOTE While the compressibility of aqueous fluids are not significantly affected by the pressure, some calibration
oils, in particular silicone oils, are affected by pressure.

2) Examples of pressurized concentric-cylinder viscometers are the Fann Model 50 viscometer equipped with rotor 1,
bob 5 (R1B5); Nordman Model 5001 equipped with rotor 1, bob 5 (R1B5); or viscometers with equivalent geometry. This
information is given for the convenience of users of this part of ISO 13503 and does not constitute an endorsement by ISO
of these products.
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SIST EN ISO 13503-1:2005
ISO 13503-1:2003(E)
b) alternative torque-only calibration
Measure according to the manufacturer's specified calibration procedure (e.g. hanging weight), which
shall be traceable to a national/international standard such as ISO, ASTM, DIN, or equivalent.
8.2.2.2.2 Operation
8.2.2.2.2.1 Instrument preparation
Pre-heat thermal bath (if equipped) to test temperature. All temperatures in this document refer to actual
temperature of the fluid.
8.2.2.2.2.2 Procedure
The following procedures shall be followed.
a) Loading, pressurizing and heating the fluid
Load the fluid to be evaluated into the viscometer immediately after the last component is added
3
according to mixing procedure. Place 52 cm of fluid in the viscometer. This volume is sufficient to fully
cover the bob. Pressurize the system with nitrogen to a minimum of 2,75 MPa (400 psi) and immediately
−1
start shearing at 100 s . When shearing of the fluid starts, define the elapsed time as zero (t = 0) and
begin heating the fluid. All actions in this paragraph shall be completed within 45 s.
Optionally, for an ambient-temperature shear ramp [described in 8.2.2.2.2 b)], elapsed time is defined as
zero (t = 0) immediately after completing this ramp, and fluid heating is begun.
At 20 min elapsed time, th
...