Guidelines - Qualification of Materials For Well Suspension and Abandonment July 2012

Guidelines on qualification of
materials for the suspension and

abandonment of wells
Issue 1
July 2012
Guidelines on qualification of materials for the suspension and abandonment of wells

Issue 1, July 2012
The United Kingdom Offshore Oil and Gas Industry Association Limited (trading as Oil & Gas UK), 2012.
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The information contained herein is given for guidance only. These guidelines are not intended to replace
professional advice and are not deemed to be exhaustive or prescriptive in nature. Although the authors
have used all reasonable endeavours to ensure the accuracy of these guidelines neither Oil & Gas UK nor
any of its members assume liability for any use made thereof. In addition, these guidelines have been
prepared on the basis of practice within the UKCS and no guarantee is provided that these guidelines will
be applicable for other jurisdictions.
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ISBN: 1 903 003 85 4

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Guidelines on qualification of materials

for the suspension and abandonment of wells
Contents
Foreword ........................................................................................................................ 4
Glossary ......................................................................................................................... 5
List of abbreviations.................................................................................................... 11
1
Introduction ........................................................................................................ 12
1.1
UK Guidelines for the suspension and abandonment of wells ..................................... 13
General considerations for qualification of new technology........................... 15

2.1
Documentation requirements ........................................................................................ 17
Functional requirements of permanent barriers .............................................. 18

3.1
Sealing .......................................................................................................................... 18
3.2
Position.......................................................................................................................... 19
3.3
Placeability .................................................................................................................... 19
3.4
Durability ....................................................................................................................... 20
3.5
Removal options and reparability concepts ................................................................ 20
Operating conditions.......................................................................................... 21
4.1
Typical conditions for wells in the North Sea ................................................................ 22
4.2
Estimating operational conditions of the permanent barrier ......................................... 23
Potential functional failure modes and root causes ........................................ 24

5.1
Shift in barrier position .................................................................................................. 24
5.2
Barrier leakage through the bulk material ..................................................................... 24
5.2.1
Fluid flow through porous media ................................................................................ 25
5.2.2
Diffusive leakage ........................................................................................................ 25
5.3
Leaks around the bulk material ..................................................................................... 26
5.3.1
External / internal stresses ......................................................................................... 28
5.3.2
Shrinkage and expansion ........................................................................................... 28
5.3.3
Chemical degradation ................................................................................................. 29
5.3.4
Creep .......................................................................................................................... 30
5.3.5
Quality of placement ................................................................................................... 30
5.3.6
Thermal expansion differences .................................................................................. 31
5.3.7
Drilling damage ........................................................................................................... 31
Material types...................................................................................................... 32
6.1
Definition of material types ............................................................................................ 32
6.2
Critical material properties related to potential failure modes ....................................... 32
Approach to defining acceptance criteria for mass transport properties ...... 34
Experimental work plan ..................................................................................... 36

8.1
Literature investigation .................................................................................................. 36
8.2
Permeation testing ........................................................................................................ 36
8.2.1
Permeability ................................................................................................................ 36
8.2.2
Diffusion ...................................................................................................................... 38
8.3
Issue 1, July 2012
Interaction with fluid ...................................................................................................... 38

8.3.1
Absorption................................................................................................................... 38
8.3.2
Leaching, corrosion and chemical resistance ............................................................ 38
8.4
Dimensional stability ..................................................................................................... 39
8.4.1
Expansion / swelling ................................................................................................... 39
8.4.2
Shrinkage.................................................................................................................... 40
8.4.3
Differential thermal expansion .................................................................................... 40
8.4.4
Creep and stress relaxation........................................................................................ 41
8.5
Mechanical testing ........................................................................................................ 41
8.5.1
Triaxial testing............................................................................................................. 42
8.5.2
Elastic modulus .......................................................................................................... 42
8.5.3
Cohesion..................................................................................................................... 42
8.5.4
Internal friction angle .................................................................................................. 42
8.5.5
Poissons ratio ............................................................................................................ 43
8.5.6
Hydrostatic compression testing................................................................................. 43
8.5.7
Unconfined compressive strength (UCS) ................................................................... 43
8.5.8
Tensile strength .......................................................................................................... 43
8.5.9
Hardness .................................................................................................................... 43
8.6
Bond strength ................................................................................................................ 44
8.6.1
Shear bond strength ................................................................................................... 44
8.6.2
Tensile bond strength ................................................................................................. 45
8.7
Fatigue life ..................................................................................................................... 45
8.8
Decomposition temperature .......................................................................................... 45
8.9
Density .......................................................................................................................... 45
8.10
Ageing testing ............................................................................................................... 46
8.11
Function test .................................................................................................................. 49
8.12
Field trial ........................................................................................................................ 51
Material types specific experimental work plans .......................................... 52

9.1
Type A: Cements, ceramics (setting) ............................................................................ 52
9.2
Type B: Grouts (non-setting) ......................................................................................... 54
9.3
Type C: Thermosetting polymers .................................................................................. 56
9.4
Type D: Thermoplastic polymers .................................................................................. 58
9.5
Type E: Elastomeric polymers ...................................................................................... 60
9.6
Type F: Formation ......................................................................................................... 62
9.7
Type G: Gels ................................................................................................................. 64
9.8
Type H: Glass ............................................................................................................... 66
9.9
Type I: Metals ................................................................................................................ 68
10
References .......................................................................................................... 70
11
Appendix 1: Chemical environment .................................................................. 72
12
11.1
Seawater and brine composition ................................................................................... 72
11.2
Oil composition .............................................................................................................. 73
11.3
Gas composition ........................................................................................................... 73
11.4
Non-native chemicals .................................................................................................... 74
Appendix 2: Radiation ........................................................................................ 75

12.1
NORM activity estimates ............................................................................................... 75
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12.2
Lost logging tools .......................................................................................................... 75
13
Appendix 3: Estimating operational pressures ................................................ 76
14
Appendix 4: Calculation of flow rates through a microannulus. ..................... 78
15
Appendix 5: Caprock properties........................................................................ 79

15.1
Typical North Sea shale properties ............................................................................... 79
15.2
Typical North Sea salt formation properties .................................................................. 79
16
Appendix 6: Flow calculations........................................................................... 80
17
Appendix 7: Diffusion calculations ................................................................... 81
18
Appendix 8: Relevant industry standards ........................................................ 83
19
Appendix 9: Cement material reference data ................................................... 86
20
Appendix 10: Shear bond strength ................................................................... 87
21
Appendix 11: Background to these guidelines ................................................ 88
If you have any feedback on these guidelines, please send your comments (referring to
the relevant paragraph number shown in the grey column) to wlcpf@oilandgasuk.co.uk.
Unfortunately the workgroup may not be able to provide individual responses to
feedback submitted. Feedback received will be used to improve the guidelines when
they are next revised.
Issue 1, July 2012

Foreword
These guidelines have been prepared to provide a reference for well-operators,

manufacturers and regulators on the qualification of materials suitable for the
temporary abandonment (suspension) and permanent abandonment of wells in
the UK and its continental shelf. The document compiles the current industry
expertise to provide guidance on how materials for suspension and well
abandonment can be qualified.
A separate Oil & Gas UK document entitled Guidelines for the suspension and
abandonment of wells [Ref 2] provides minimum criteria to help ensure full and
adequate isolation of formation fluids, both within the wellbore and from surface
or seabed. This will assist well-operators to comply with the UK Offshore
Installations and Wells (Design and Construction, etc) Regulations (SI
1996/913) (hereafter referred to as DCR). Regulations are goal setting in nature
and lay down the standard that should be achieved. In essence, DCR requires
the well-operators to prevent, on a permanent basis, escape of fluids from the
well. Allowance must be made for deterioration of some components of the well
over time.
Cement is currently accepted as the primary material for permanent barriers in

well abandonment, principally on the basis that it is considered to have similar
properties to the rock that it is replacing. However, cement has operational
limitations, and alternative materials are being proposed and developed by the
industry. Although there are potentially many advantages in using such
materials, they have currently seen little or no application in well
abandonments. One significant reason for this is that well abandonment has an
eternal perspective, and uncertainty with regards to long-term integrity of
alternative materials acts as a disincentive for their use. The aim of this
document is to stimulate consideration of a broader range of materials for
abandonment.
The deployment of a novel barrier material for suspension or abandonment of

wells should follow a sequence of phases from development, qualification,
production, storage, transport, installation and verification. Using this sequence,
this document covers the qualification steps to ensure that the considered
material performs the envisaged function. Product development, production,
storage, transport and installation are outside the scope of this document. Also
outside the scope of the document is the qualification for health, safety and
environmental acceptance.
When comparing UK requirements to those of other countries, there are few

differences with NORSOK in Norway. Other countries may only refer to cement
or indicate that an abandonment material must be equivalent to cement. Some
countries may also accept mechanical devices as permanent barriers without
further specification.
This is the first issue of these guidelines. It is envisaged that updated versions
will be released on a three-yearly cycle.
Issue 1, July 2012

Glossary
8
9
anoxic: A term used to refer to conditions where oxygen is absent.
10
bailer: Container with plugging material that is lowered into a well on wireline to
deliver a small amount of plugging material by remotely opening the container
at depth. In this context it is more commonly known as a dump bailer that
implies the functionality of the equipment.
11
barrier material: Material used in a well to provide a seal as part of a

permanent barrier.
12
barrier plug: A volume of barrier material used as either a temporary barrier

or permanent barrier.
13
borehole: Hole drilled in the earth crust for extracting fluids from rock
formations. Other purposes can include injection, heat exchange or gather data.
The borehole can also include the open hole or uncased part of a well.
Borehole may refer to the internal diameter of the well and also the formation or
rock face that bounds the drilled hole. Also, see well.
14
branch: See sidetrack.
15
bridge plug: Traditionally, a device that can be set in a well to isolate the lower
part of the wellbore. Bridge plugs may be classified as either permanent or
retrievable and can also be provided as an inflatable device. In the context of
well abandonment, a bridge plug can be used as a mechanical device to
provide a solid base for setting a permanent barrier such as a cement plug.
16
brine: Water saturated or containing high concentrations of salts, in particular,

sodium chloride, potassium chloride and calcium chloride.
17
caprock: The general term for the rocks that trap hydrocarbons in the reservoir.
Another term used for these types of rocks is seal.
18
carbon dioxide: A gas which occurs with hydrocarbons in some geographical

areas. Deterioration of components in a well can occur from contact with
carbonic acid, which is formed when carbon dioxide dissolves in water or there
is moisture in the environment. The deterioration is normally referred to as
sweet corrosion and typically results in deep pitting and material loss where
there is exposure to carbonic acid. There are a number of different quantitative
models available to assess the loss of material, however these are partial
models using selective parameters.
Issue 1, July 2012

19
casing or casing string: An assembled length of long hollow cylinders, usually

steel in a quenched and tempered condition with threaded connections,
configured to suit a specific wellbore. The sections of pipe are connected and
lowered into a well, then cemented in place to provide a conduit for fluids to be
conducted. Casing is also defined as Oil Country Tubular Good (OCTG) with
sizes ranging from 4-1/2 inches to 20 inches in diameter. Casing can be divided
into different types which perform different functions. The different types are
typically classified as (in order of decreasing diameter); conductor (also known
as stove pipe), which is the outermost string of casing through to surface
casing; intermediate casing; and production casing. The names assigned to the
different types of casing strings also imply the functionality of the particular
casing string.
20
casing annulus: The space between the casing and the next larger casing or
rock.
21
cement slurry: A suspension of cement and possibly other granular material in

water which flows as a liquid.
22
coiled tubing: A long continuous length of pipe wound on a spool. The pipe is
straightened prior to lowering it into a wellbore and rewound to coil the pipe
back onto the transport and storage spool. Depending on the pipe diameter
(typically 1 inch to 4-1/2 inches) and the spool size, coiled tubing can range
from 2,000 feet to 15,000 feet or greater length. As a well intervention method,
coiled tubing techniques offer several key benefits over alternative well
intervention technologies. The ability to work safely under live or pressurised
well conditions, with a continuous string, enables fluids to be pumped at any
time regardless of the position or direction of travel. This is a significant
advantage in many applications. Installing a multicore electric line logging cable
within the coiled tubing further enhances the capability of a coiled tubing string
and enables relatively complex intervention techniques to be applied safely.
23
completion: A generic term used to describe the assembly of a string of tubing

that includes a variety of different subcomponents, which are selected
depending on the functional design of a well, that are required to enable the
safe and efficient operation of the well. This term can also be used as an
all-encompassing term or alternatively as constituent parts such as lower
completion, intermediate completion and upper completion.
24
completion fluid: A solids-free liquid that fills the wellbore during the
completion phase of the well construction process. The fluid is meant to control
a well, should downhole hardware fail, without damaging the reservoir or
completion. Completion fluids are typically brines (e.g. solutions of chlorides
and bromides), but in theory could be any fluid of proper density and flow
characteristics such as seawater or base oil. Also known as kill weight brine
as the bottomhole hydrostatic pressure in the well bore (of the completion fluid)
is greater than the exposed formation pressure.
25
creep: Permanent deformation resulting from prolonged application of stress

below the elastic limit.
26
diffusion: A process where a substance is transported from a region of high

concentration to a region of lower concentration.
Issue 1, July 2012

27
diffusive leakage: The release of fluid above a barrier as the result of

diffusion.
28
drill cuttings: Solids removed from a well while drilling.
29
drilling fluid: Fluid that fills the wellbore during the drilling phase of the well
construction process. Consists of any of a number of liquid and gaseous fluids
and mixtures of fluids and solids (as solid suspensions, mixtures and emulsions
of liquids, gases and solids). Also known as "mud which is in general usage,
although some individuals prefer to reserve the term "drilling fluid" for a more
sophisticated and well-defined "mud". Can also be referred to as drill-in-fluid
which is a special fluid designed exclusively for drilling through the reservoir
section of a well.
30
drill pipe: A long hollow cylinder, usually steel in a quenched and tempered
condition, with threaded connections which are called tool joints. An assembled
length of drill pipe which connects the drilling rig surface equipment with a
bottom hole drilling assembly and drill bit is collectively known as a drillstring.
The drillstring is used to pump drilling fluid to the drill bit for driving a revolving
drill bit for drilling wells.
31
ductile: A material characteristic relating to the ability to deform plastically, and

thus be drawn out into a wire.
32
dynamic viscosity: A measure of the resistance of a fluid to deformation by

either shear or tensile stress. Units = Pa.s.
33
enhanced oil recovery: Techniques employed to increase the amount of oil

which can be extracted from a field. This generic term can also be more
specifically classified as secondary EOR or tertiary EOR.
34
fluid: Within the context of this document a fluid is a substance in either the
liquid or gaseous state.
35
flux: The rate of flow of a fluid through a unit area.
36
formation: Rock present in the crust of the earth.
37
geopolymer: Alkali-activated aluminosilicate cement.
38
hydrogen sulphide: An extremely poisonous gas which is produced during the

decomposition of organic matter and occurs with hydrocarbons in some
geographical areas. Hydrogen sulphide can also be generated by sulphatereducing bacteria. Mercaptons can also be a by-product of the interaction of
hydrogen sulphide with hydrocarbons. A well that is contaminated with
hydrogen sulphide is often referred to as a sour well and should be designed
for sour service. Hydrogen sulphide can cause sulphide stress cracking of
metals; however this can be addressed with the use of corrosion-resistant
alloys. Materials for use in a hydrogen sulphide environment can be controlled
by the standard NACE MR0175 / ISO 15156.
Issue 1, July 2012

39
liner: A casing string that does not extend to the top of the well, but instead is
anchored or suspended from inside the bottom of the previous casing string.
The device used to anchor or suspend a liner from a casing string is known as a
liner hanger. The liner can be fitted with special components so that it can be
connected to the top of the well at a later time if required.
40
LSA scale: See NORM.
41
mechanical plug: a device used to produce a seal in a casing through the

application of forces by mechanical means.
42
mud: See drilling fluid.
43
naturally occurring radioactive material (NORM): Substances encountered

in the environment which contain native, naturally occurring radioactive
isotopes. NORM is sometimes encountered as scale formed in parts of a well,
where it may have become enriched with radioactive material as a result of the
processes it has undergone. NORM is sometimes referred to as Low Specific
Activity (LSA) scale.
44
non-native materials: Materials introduced into or around the well as a result

of production activities.
45
packer: A device used in well completion to isolate the annulus from the
production casing, enabling controlled production, injection or treatment. A
packer assembly incorporates a means of securing the packer against the
casing or liner, and a means of creating a reliable seal to isolate the annulus,
typically by means of an expandable elastomeric element.
46
permanent barrier: A verified barrier that will maintain a permanent seal. A

permanent barrier must extend across the full cross section of the well and
include all annuli.
47
permanent barrier material: Material used in a well to provide a seal as part of

a permanent barrier.
48
permeation: The movement of a substance through a material. Permeation can

occur under either a pressure differential or a concentration differential.
49
permeability: a measure of the ability of a porous material to allow transport of

fluids.
50
permeable zone: Any zone in the well where there is the possibility of fluid
movement on application of a pressure differential.
51
sidetrack: To drill a secondary well away from an original well or a donor well.
A sidetracking operation may be done intentionally or may occur accidentally.
Intentional sidetracks might be used to bypass an unusable section of the
original well or to explore a geological feature nearby. In the bypass case, the
secondary well is usually drilled almost parallel to the original well, which may
be inaccessible due to problems encountered during the well construction
process. It is also possible to have multiple sidetracks in a single well, each of
which might be drilled for a different reason. This term can also be used to
describe part of a multilateral well where multiple wells or boreholes originate
from one donor well or borehole.
Issue 1, July 2012

52
simulated in situ fluid: A fluid comprising a mixture of water, hydrocarbons

and gases in proportions which mimic the composition of a downhole fluid.
53
suspension: Also referred to as temporary abandonment. Action taken prior

to leaving the well to ensure adequate isolation of permeable zones, fluids and
pressures in any well that will be re-entered or abandoned at a later date.
54
sour well: See hydrogen sulphide.
55
sweet well: A well containing relatively high concentrations of carbon dioxide.
56
temporary barrier: A verified barrier that is designed to maintain a seal over a

finite period of time for the purpose of suspension. A temporary barrier is not
required to extend across the full section of the well and include all annuli.
57
through-tubing: Activity in which material is placed downhole using tubing or

coiled tubing.
58
tubing: See casing.
59
viscous pill: In the context of well abandonment a pill can be used to provide a
nominally quasisolid base for setting a permanent barrier such as a cement
plug. Pills can take the form of viscous pills, whose viscosity acts to limit
mobility, viscous reactive pills whose viscosity derives from a chemical reaction
when in contact with cement or other substances. A pill will typically be
weighted of suitable density to allow it to locate itself at the correct depth.
60
well: A hole drilled into the Earths surface to extract petroleum oil and fossil
natural gas. A well includes the original drilled hole (the wellbore), any
sidetrack from it and any hole section. Also see borehole.
61
wellbore: See well.
62
wireline: Deployment method of lowering into and retrieving tools and devices
from a well. A generic term used to describe well intervention operations
conducted using a single-strand or a multistrand wire or cable in wells. Although
applied inconsistently, the term is commonly used in association with electric
logging and cables incorporating one or several electrical conductors leading to
the terms monoconductor cable or multicore electric line logging cable.
Similarly, the term slickline, or piano wire, is commonly used to differentiate
operations performed with single-strand wire or braided lines.
63
work string: A generic term used to describe a tubing string used to convey a
treatment or for well intervention activities. Both coiled and jointed tubing strings
are referred to as work strings.
Issue 1, July 2012

64
Interpretation
In these guidelines:
reference to any legislation or publications includes a reference to that
legislation, publication as may be amended, extended or re-enacted from
time to time;
reference to the singular shall include the plural and vice versa;
reference to include means including but not limited to;
the headings are used for convenience only; and
regard has only been made to the jurisdictions within the UK.
10
Issue 1, July 2012

List of abbreviations
65
66
API
American Petroleum Institute
ASTM
American Society for Testing and Materials
CH4
methane
CO2
carbon dioxide
CT
computer tomography
DCR
Offshore Installations and Wells (Design and Construction, etc)

Regulations 1996 (SI 1996/913) which is commonly known as the
Design and Construction Regulations
DSC
differential scanning calorimetry
DTA
differential thermal analysis
EOR
enhanced oil recovery (see Definitions)
H2S
hydrogen sulphide
ISO
International Organization for Standardization
ISRM
International Society for Rock Mechanics
LSA
low specific activity
MRI
magnetic resonance imaging
NACE
National Association of Corrosion Engineers
NMR
nuclear magnetic resonance
NORM
naturally occurring radioactive material
ppmv
parts per million by volume
SEM
scanning electron microscope
SIF
simulated in situ fluid
TGA
thermogravimetric analysis
UCA
ultrasonic cement analyser
UCS
unconfined compressive strength
UKOOA
United Kingdom Offshore Operators Association now known as

Oil & Gas UK
Issue 1, July 2012
11

67
Introduction
68
Wells that have been used to explore or develop hydrocarbon accumulations

will at some stage require abandonment. This involves placement of barriers in
the well to isolate formations from each other and from surface. This is referred
to as permanent abandonment if there is no intention to ever re-enter the
abandoned part of the wellbore. Where there is an intention to re-enter, it is
referred to as temporary abandonment or suspension. Suspension is
typically short term (a matter of months). Long-term suspension should be the
exception rather than the rule.
69
A simplified schematic of a permanently abandoned well is shown in Figures 1

and 2. It is stressed, however, that wells differ in construction and operation and
that the abandonment must reflect this. It should also be emphasised, that the
barriers placed during abandonment may not exclusively be cylindrical barriers
within the casing for instance, it may be necessary to place barriers in the
annulus between the caprock and the casing.
70
Portland cement is currently the most used barrier material in permanent well
abandonment. This is because it is considered to have similar properties to the
caprock that it is replacing. In existing abandonments, cement is functioning as
required in most cases, but there are operational limitations and situations in
which cement may not be the most appropriate material. The aim of this
document is to stimulate consideration of alternative materials for
abandonment.
71
This document covers materials that will cause the sealing action, but not the
construction of mechanical devices such as packers or mechanical plugs, nor
the placement technique. This document does not cover formation damaging
materials. Such materials are currently available, but are not included in existing
guidelines. However, they may be included in subsequent versions of this
document.
72
BEFORE
AFTER
Caprock
for zone B
Zone B
Water bearing
Caprock
for zone B
permanent
barrier to
zone B
Zone B
Water bearing
Casing
Cement
Caprock
for zone A
Zone A
Secondary
permanent barrier
to zone A
Caprock
for zone A
Oil and Gas
Zone A
Primary permanent barrier

to zone A
Oil and Gas
Figure 1. Simplified schematic of the abandonment of a well by placement of

permanent barriers. See Figure 2 for a close-up of a barrier. In case of
suspension there will generally be no casing cut or removed.
12
Issue 1, July 2012

Permanent Abandonment Barrier (red dashed envelope)
73
Best practices
Restoring the caprock
Barrier elements
Sealing
abandonment plug
Tubing sealed with
cement, in cement
Height of 500 ft
MD, containing at
least 100 ft MD of
good cement.
Plug depth
determined by
formation
(impermeability
and strength) and
primary
cementation
Casings, tubing
embedded in
cement
Sealing primary
cementations
Pipe stand-off
Support to prevent
cement movement,
slumping and gas
migration while setting
Good bond,
clean
surfaces,
water wet
Formation:
impermeable and
adequate strength
to contain future
pressures
Figure 2. A permanent barrier is an envelope (red dashed line) that

encompasses a number of barrier elements (orange boxes), which all need to
seal. Cement is assumed. Recommended or best practices (blue boxes) are
indicated.
74
1.1 UK Guidelines for the suspension and abandonment of wells
75
In the UK, well design and construction both onshore and offshore is regulated
by the Offshore Installations and Wells (Design and Construction, etc)
Regulations (SI 1996/913) (hereafter referred to as DCR).
76
Regulation 13 General duty of the DCR states that:

1. The well-operator shall ensure that a well is so designed, modified,
commissioned, constructed, equipped, operated, maintained, suspended
and abandoned that
a. so far as is reasonably practicable, there can be no unplanned escape of
fluids from the well; and
b. risks to the health and safety of persons from it or anything in it, or in
strata to which it is connected, are as low as is reasonably practicable.
77
Guidance on DCR is available [Ref 1].
78
Regulation 15 with a view to suspension and abandonment of DCR states

that:
The well-operator shall ensure that a well is so designed and constructed that,
so far as is reasonably practicable
a. it can be suspended or abandoned in a safe manner; and
b. after its suspensions or abandonment there can be no unplanned escape of
fluids from it or from the reservoir to which it led.
Issue 1, July 2012
13

79
Through Oil & Gas UK (formerly known as UKOOA), the industry has compiled
the Guidelines for the suspension and abandonment of wells [Ref 2] which
provide minimum criteria as a means to achieve the specific regulations
detailed in DCR.
80
The Guidelines for the suspension and abandonment of wells state that the
main characteristics of permanent barrier materials should be as follows:
very low permeability - to prevent flow of hydrocarbons or overpressured
fluids through the barrier;
long-term integrity - long-lasting isolation characteristics of the material, not
deteriorating over time;
non-shrinking - to prevent flow between the barrier-plug / casing annulus;
ductile - non-brittle material; to accommodate mechanical loads and
changes in the pressure and temperature regime (conversion of producers
to water injectors, steam injection, unconsolidated formations etc);
resistance to downhole fluids and gases (CO2, H2S, hydrocarbons etc); and
able to bond to the casing or formation in which it is placed.
81
On the subject of alternative (non-cement) plugging materials, the guidelines

add the following:
Cement is currently used in wells as the prime material for abandonment
purposes. This does not preclude the use of other materials. Alternative
materials should, in principle, conform to the requirements above. The longterm integrity of materials should be documented. Once placed, there should be
a means by which the barriers can be verified.
82
The guidelines also state that:

The downhole placement technique of the plugging material is extremely
important, especially in cases of through-tubing applications. Allowances will
have to be made on the volumes to cater for contamination and shrinkage. A
support (such as a bridge plug or a viscous pill) to prevent slumping of the
cement slurry, is recommended for all cement plugs.
83
14
Whilst the Guidelines for the suspension and abandonment of wells have been
used as a means of steering the development of the guidance in this document,
it should be stressed that, in the case of certain properties, the approach has
been taken to require materials displaying appropriate performance in service,
rather than specific characteristics.
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84
General considerations for qualification of new

technology
85
Whilst a permanent barrier must be verified in the field, placement of such a

barrier must be preceded by qualification of the materials used. This section
represents general requirements related to the qualification of new technology,
as defined in the Det Norske Veritas document Qualification procedures for new
technology (DNV RP-A203, 2001) [Ref 3]. An outline of the process (with some
modification) is shown in Figure 3.
86
The first stages of the qualification process involve establishing a plan for
qualification. This plan should control the subsequent qualification activities.
The qualification should be based on the following philosophy:
The qualification process should be based on a systematic approach.
Possible failure modes should be identified, and their relevance should be
determined based on their risk, i.e. the combined probability and
consequences of a failure mode occurring. Risk in this context is related to
the functionality of the new permanent barrier material.
A programme of measurements and tests should be devised an
experimental work plan - which is appropriate to evaluate the suitability of
the material for its use as a barrier material, giving consideration to the
materials in contact with the barrier.
Theoretical analysis and calculations should, when practical, be used as the
main tool to record fulfillment of the specifications and margins against
failure. Theoretical calculations should be verified by tests, including a
function test (see Section 8.11).
The experimental work plan used as the principal means of demonstrating
and documenting that manufacture and deployment fulfil the specifications.
87
Furthermore, the following principles should control the qualification process:

Specifications and functional requirements should be quantitative.
The margins for capacities and margins against failure should be
established based either on recognised methods, standards, or on
combinations of all uncertainties used in the data, operation, calculations
and tests.
When experience is used as proof of fulfilment of the specifications and
reasonable margins, this should be documented.
The limiting material and functional parameters to be used in the analysis
should be identified through tests or referenced to recognised literature.
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88
Define Qualification Basis

Identification of Failure Modes
Ranking of Failure Modes in Terms

of Risk
Data Collection
Selection of Qualification Methods
and Planning
Assessment of Probability of
Successful Evaluation
Documentation
Analysis and Testing
Laboratory
Testing
Function Test
(larger scale)
Reliability Analysis
Documentation
Figure 3. Process for the qualification of new technology [Ref 3].
89
16
Confidentiality of the technology should not limit the information made available
for the qualification. These guidelines assume that confidentiality between
parties is arranged by contracts to that purpose. The available documentation
and insight into the qualification process may follow three alternatives:
An open qualification scheme - all information is available.
The qualification documentation is made available to a third party
recognised by the involved parties.
The original qualification documentation is not accessible. Full function and
endurance tests according to the specifications must document the
qualification, in addition to the suppliers statement of qualification. This may
imply more extensive testing than the former. These tests must demonstrate
acceptable margins for all conditions. It may imply testing of a sufficient
number of batches to develop statistically representative data.
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90
91
It is recommended that the qualification method, qualification steps and tests

are agreed beforehand with potential users and relevant regulators.
2.1 Documentation requirements
92
With reference to DNV RP-A203 [Ref 3], the available documentation related to
the qualification process should, when applicable, comply with the following:
description and specification;
material specifications;
quality assurance plan; and
detailed drawings of items used in the qualification.
93
The documentation of the qualification should include the following, when

applicable:
Design criteria:
references with justification to applied standards, rules and regulations;
selection of types of tests with justification;
selection of test parameters with justification; and
expected outcome of each test, with quantified acceptance levels.
Documentation of key items in the qualification process:
description and justification of methods (experience, analysis and tests)
applied for qualification;
document tests performed, conditions and parameters used, with results,
including failures with analysis;
values of key parameters and conditions at the start of a test are to be
captured;
resulting margins to failure modes;
limit values (maximum or minimum) functions from analyses and tests;
and
system reliability.
Analysis:
failure mode analysis, including specification of personnel competence;
list of all assumptions made in the failure mode assessment;
conclusions on operating envelope of the material;
statement of conditions or parameters that were not tested or evaluated
in the qualification process; and
minimum lifetime estimate describing appropriate extrapolation technique
and assumptions.
Manufacturing and installation:
material certificates;
manufacturing records;
personnel qualification record;
installation records; and
material samples taken and kept.
Revisions:
records of all document revision including content of revision.
94
95
96
97
98
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99
100
101
18
Functional requirements of permanent barriers

A permanent barrier has to fulfil a number of functions, which are discussed
below. Functional requirements of temporary barriers do not differ from those of
permanent barriers except possibly for a relaxed time scale of required
durability.
3.1 Sealing
102
The main function of a permanent barrier is to provide a seal against movement

of fluids. However, permeation of some kind is possible through most materials.
Such fluid movement follows well understood natural processes. Within the
context of permanent barrier materials it must, therefore, be recognised that it is
inevitable that a fluid within the well will ultimately migrate past a barrier, albeit
at a low rate.
103
Thus, appropriate barriers are those through which the rate of permeation is
acceptably low. The approach taken in this document is to require that the
barrier permits leakage of fluids at the same or a lower rate than the caprock.
The permeability of caprock is typically within the range 0.001-1 microdarcy.
However, good quality cement (typically with a permeability of 10 microdarcy) is
deemed acceptable on the basis of historical industry experience, and on the
grounds that barrier length is a controllable parameter (as long as it is opposite
the caprock) and the cross sectional area is considerably smaller than that of
the caprock. A permanent barrier requires:
continuous material, or sequence thereof, with low-permeability; and
an appropriate length along the well bore.
104
The rate of permeation in this context is controlled by a number of factors,

including:
Fluid flow through connected porosity. In this case the driving force for fluid
transport is a pressure differential.
Diffusion processes. The driving force for transport is a concentration
difference.
Conduits due to defects in the barrier material, such as cracks or channels.
The driving force for fluid transport is a pressure differential.
Conduits at interfaces between the barrier material and surrounding
materials, e.g. casing, liner, tubing, rock formations. The driving force for
fluid transport is a pressure differential.
105
These factors, plus the length of the barrier, will control the lag time before a
specified fluid is released above the barrier. Therefore, the minimum length of
barrier will vary depending on the material properties, and the placement
technique should be selected based on its capability to place such a volume of
material. Fluids will typically include oil, gas, CO2, H2S, water and brine, any of
which may contain corrosive components.
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106
107
3.2 Position
Once placed, the position of the barrier should not move, either along the well
bore or in a lateral direction. This means, for instance, that the barriers should
not be pushed upwards by pressure developing below. The barrier material is
required to remain attached to interfaces it has been placed against. This is
achieved through sealing stresses normal to the casing (Figure 4), friction
stress, bonding at the interface, weight and dimensional stability, or a
combination of these.
108
Figure 4. Forces acting to maintain the seal and position of a barrier.
109
3.3 Placeability
110
It is a requirement that the permanent barrier material can be placed in a

wellbore at depth and is subsequently able to perform its required function [Ref
2].
111
The material should have appropriate properties that allow it to displace the
existing fluids and form a continuous sealing medium, even when taking its
inevitable contamination into account. The material may be circulated in place
to replace the present fluid. This will require a work string, such as drillpipe,
tubing or coiled tubing. The work string may be left in place and become part of
the barrier. If suitable, a gravity-based placement may be deployed using a
bailer device and multiple wireline runs.
112
Where a barrier material undergoes a transformation from a liquid to a solid,

this period of transformation must be sufficiently short to prevent escape of fluid
and unacceptable disruption of the barrier.
113
Wells may be positioned at an angle to the vertical, and the placement

technique employed should take this into account.
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19

114
A means of verifying that the placement of the permanent barrier has been
successful is required.
115
For recommendation of placement techniques refer to the Guidelines for the

suspension and abandonment of wells [Ref 2].
116
117
The barrier material should not degrade such that its sealing capability or
position is compromised. For temporary abandonment an anticipated timescale
may be specified. Permanent well abandonment has an eternal perspective,
meaning that the mindset for design is in terms of geological timescales, which
span millions of years. It will not be possible to quantify such a time
requirement, and it is clearly not feasible to qualify materials for this timescale.
118
In order to define testing criteria against a quantified service life, a service life of
an arbitrary number of a million days (circa 3,000 years) is proposed in the
context of this document. This is of the same order of magnitude as
requirements for the storage of CO2, which refer to timescales of thousands of
years, although it has been suggested that an expectation of more than 30
years will be difficult to prove for most materials [Ref 4].
119
The estimation of long-term performance through ageing testing is discussed in

greater detail in Section 8.10.
120
121
20
3.4 Durability
3.5 Removal options and reparability concepts

A key objective of permanent well abandonment is that re-entry into the well
should be unnecessary. However, in the rare event that a leak through a barrier
would develop, there should be a method to remove the barrier(s) in order to
remedy the leak. This is in line with the mindset in CO2 storage projects.
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123
124
Operating conditions
After placement and activation, the permanent barrier material will have to
withstand external loadings, and variations in these loadings, without losing its
functionality as part of a permanent barrier. Likely operating conditions are
listed below. Qualification will be limited to the stated envelope of each of these
parameters.
Pressure and variation: Pressure will change during the production life of
a field or due to recharging of a depleted reservoir to original pressure.
Pressure in the wellbore may change if suspended particles settle and the
fluid changes weight. Wellbores under barriers may eventually become
pressurised due to formation and / or wellbore connectivity with deeper
strata. enhanced oil recovery (EOR) of an existing field or redevelopment of
an abandoned field may require injection of fluids, possibly to pressures
exceeding original pressures. Fields may be charged for storage of gas or
CO2. During abandonment operations (e.g. pressure / inflow testing, fluid
change) rapid decompression may damage certain barrier materials.
Temperature and variation: Temperature will change during the

production life of a field, but follows geological patterns when left
undisturbed. Redevelopment of an abandoned field may also lead to
temperature changes, e.g. during steam injection. Thermal changes may
also result from fluid injection, gas storage or CO2 injection in previously
abandoned fields.
Mechanical stresses and variation: Naturally occurring formation creep,

subsidence or tectonic forces may act on a permanent barrier. Additionally,
changes in temperature will cause expansion and contraction. Where
materials with very different coefficients of thermal expansion are in contact,
particular problems may be encountered in environments where
temperatures change, as the differential magnitudes of volume change can
create significant stresses. For instance, casings may expand or contract
due to temperature and pressure variation, causing mechanical forces to act
on the barrier material. Loads on casings may change from tension to
compression during abandonment. Rapid short-term stresses may also be
created by explosive techniques used in wells to sever or perforate tubular,
tagging with the drillpipe for verification and pressure testing.
Chemicals: Barrier materials may be exposed to native substances such as

hydrocarbons, CO2, H2S and brine, as well as non-native chemicals deriving
from production. Further details of the chemical nature of downhole
environments are provided in Appendix 1. Such chemicals may either
undergo reactions with the barrier material which lead to deterioration, or
leach constituents from the barrier, thus compromising its integrity.
Operating temperatures and pressures may influence rates of reaction and
leaching.
125
126
127
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21

Water: Water may cause swelling of polymers, clays, etc. Osmotic

processes may also cause dimensional instabilities. Degradation of
materials through leaching or other dissolution processes may occur. If
water contains more than 50,000 mg/L of dissolved solids, it is a brine.
Brines can contain a range of types and concentrations of salts, which may
contribute towards chemical degradation. Lack of water may also be an
issue, since drying of some materials will cause alteration of properties such
as shrinkage.
Oxygen: Anoxic conditions are a normal state in the well. Low levels of
oxygen may be initially present, but deplete due to chemical processes.
Biological: Various microorganisms with the ability to digest barrier

materials or which produce substances capable of attacking them may be
present. These include sulphate reducing bacteria, which convert sulphates
and sulphites to H2S. Bacteria may be introduced into the well as a result of
injection of seawater or drill cuttings, or through circulation of seawater.
Radiation: Radiation loading is generally low underground. NORM

deposition in tubulars may be present. Lost neutron logging tools are rarely
used, but may occasionally be present. Typical radiation levels from both of
these types of source are listed in Appendix 2.
Light and UV radiation: There is no visible light or UV radiation down hole.
128
129
130
131
132
133
134
22
The well abandonment may be only partial the upper part of the hole may be
reused for drilling a new branch or sidetrack. The further operation of the field
may influence the loading conditions.
4.1 Typical conditions for wells in the North Sea
135
There is a wide variation of downhole conditions across fields and wells in the
North Sea. The permanent barrier material used should be appropriate for the
conditions of a specific well. However, in an attempt to define an envelope for
typical conditions, Table 1 is provided. This defines conditions associated with
different vertical reservoir depths.
136
Well conditions can also be defined as either sour or sweet, with the fluids in
sour wells having high H2S concentrations. Sweet wells are those that do not
contain high concentrations of H2S, but can contain a high concentration of
CO2.
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Typical Conditions
137
Well type and depth range
Initial pressure
range at reservoir,
MPa (psi)
Temperature range
at reservoir
Temperature range
at surface,
1,500 to 3,000
15 to 35
40 to 100
0 to 10
(5,000 to 10,000)
(2,000 to 5,000)
(104 to 212)
(32 to 50)
3,000 to 4,500
30 to 60
80 to 150
0 to 10
(10,000 to 15,000)
(4,000 to 9,000)
(176 to 302)
(32 to 50)
4,500 to 6,000
40 to 70
130 to 150
0 to 10
(15,000 to 20,000)
(6,000 to 10,000)
(266 to 302)
(32 to 50)
3,000 to 6,000
70 to 105
130 to 200
0 to 10
(10,000 to 20,000)
(10,000 to 15,000)
(266 to 392)
(32 to 50)
3,000 to 6,000
105 to 140
200 to 300
0 to 10
(10,000 to 20,000)
(15,000 to 20,000)
(392 to 572)
(32 to 50)
m (ft)
Shallow
Medium
Deep
HPHT
Ultra
HPHT
C (oF)
C (oF)
Table 1. Typical North Sea well conditions.
138
4.2 Estimating operational conditions of the permanent barrier
139
Prior to characterising a material for a given abandonment application, it is

necessary to establish the likely operational conditions during the lifecycle of
the well and beyond.
140
Wells may be used for future purposes not anticipated prior to abandonment. It
is the well-operators responsibility to estimate the likely conditions based on
current knowledge of a wells future operation, rather than to attempt to predict
unknown future events.
141
The anticipated well status will have to be taken into account and documented
(e.g. placement method, deposits, fluids). This will include an evaluation of all
the parameters listed previously in this section. Information may be obtained via
a number of means including actual field data; generalised field data or
calculations. A suggested method for estimating the stresses acting on a barrier
under simple pressure conditions is outlined in Appendix 3. The relevant
parameters should then be addressed by the experimental work plan.
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142
Potential functional failure modes and root causes
143
A permanent barrier material may fail in such a way that its functionality is
compromised. A number of failure modes are identified and described in this
chapter:
shift in barrier position;
barrier leakage through the bulk material; and
barrier leakage around the bulk material.
144
Placement of a barrier in the field must be accompanied by a documented

method for assurance that a barrier performs its intended function. The
objective of this verification is to ensure that none of the failure modes are
present. Methods for verification will depend on material properties, placement
technique used and well configuration. The methods employed should be
documented.
145
5.1 Shift in barrier position
146
The position of a permanent barrier in the borehole is important. A permanent

barrier should remain at its intended vertical position and retain a seal.
Excessive movement of the permanent barrier upwards or downwards may
render it ineffective in the long term. Details of requirements for the positioning
of barriers are given in the Oil & Gas UK Guidelines for the suspension and
abandonment of wells [Ref 2].
147
Regulations in some countries may require that a barrier is placed across

perforations. Upwards or downward movement will expose the perforations.
Regulations may also require that a barrier is placed across the top of a liner or
across a cut casing (casing stump). In these cases, position-holding of the
barrier material remains essential.
148
149
24
5.2 Barrier leakage through the bulk material

The generic behaviour of mass transport through a barrier is shown in Figure 5.
This depicts the flux of fluid into, and the resulting outflux from, the barrier. A lag
time is common in most situations. Different physical processes may govern
behaviour, including absorption, adsorption and displacement of resident fluid.
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150
Figure 5. The principle of permeation of a fluid through a material.
151
152
As previously discussed in Section 3.1, there will be inevitable permeation of

fluids. Permeation refers to the transport of a fluid through the barrier material.
Permeation requires a physical or chemical driving force, whilst the barrier
material will provide resistance to fluid transport. The level of resistance will
depend on the materials properties under a given set of operating conditions.
Permeation will generally follow two mechanisms fluid flow and diffusion.
5.2.1
Fluid flow through porous media
153
Fluid flow will occur in materials which contain porosity. The driving force of fluid
flow is a pressure difference between the well interior and the top of the barrier,
with a larger differential producing a higher rate of flow. Flow may also be
driven by fluid buoyancy effects, where forces arise from fluid below a barrier
possessing lower density than that above.
154
The material property governing the rate of flow is permeability, expressed in

darcys, which is a function of the volume of porosity, pore size distribution,
interconnectivity and the number of fluids and their saturation. Where multiple
fluids are present within the pores of a material (gas / liquid, mixtures of
immiscible liquids) the permeability of an individual phase is referred to as
relative permeability. This will typically be lower than for the situation where
the fluid is present in isolation.
155
156
5.2.2
Diffusive leakage
Diffusive leakage is leakage resulting from fluids diffusing through the barrier.
The driving force for diffusion is a difference between the concentration of a
fluid above and below the barrier, with a higher difference producing a greater
rate of diffusion. The material property that governs the rate of diffusion is the
diffusion coefficient, expressed in m2s-1 or similar.
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157
26
5.3 Leaks around the bulk material
158
Whilst breakthrough and outflux are inevitable for any barrier, the barrier will
have failed in its function if the lag time is shorter and / or the rate of outflux is
faster than intended. The main reason for such an occurrence is the formation
of a leak.
159
A leak is a breach of integrity which passes completely through the barrier.

Such a breach can take the form of a crack or channel development and may
be present from the start of placement or develop over a long or short period of
time.
160
Failure modes include:

debonding (formation of a micro-annulus);
dissolution e.g. leaching; and/or
cracking.
161
Root causes can include:

external/internal stresses exceeding strength limits;
shrinkage and expansion;
chemical degradation;
creep;
poor quality of placement;
thermal expansion differences; and/or
drilling damage.
162
Some modes of barrier failure are shown in Figure 6. The formation of a breach
will normally lead to an increase in the flux of fluid passing through the barrier
(Figure 7). The various root causes are discussed below.
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163
Interface casing/cement
(micro-annulus, channel)
well
casing
cement
fill
formation
rock
Interface casing/cement
(micro-annulus)
(wax, scale, oil, dirt,etc)
barrier
Bulk permeability
(connected pores, cracks,
channels)
Leak in casing (connection)
(corrosion, deformation)
channel
Annulus cement
(connected pores, cracks)
Oil & Gas UK WG4b
Interface rock/cement
(micro-annulus, channel)
6
(mudcake, cuttings, oil, etc)
Figure 6. Barrier failure modes. Modified from [Ref 5].
164
Figure 7. Permeation of a fluid material or gas through a barrier where a breach

occurs. The time of the breach may vary, e.g. immediately.
Issue 1, July 2012
27

165
External / internal stresses
166
The external stresses acting on a permanent barrier have been discussed in

Section 5. Where the barrier is a solid monolith, and stresses exceed the
strength of the barrier or the strength of any bond between the casing and the
barrier, failure will occur. Where failure of the material itself occurs, cracks will
form in the material. These cracks can exist over a range of dimensions with
widths in the millimeter to micrometer scale.
167
Where there is a failure of the casing-barrier bond, debonding will occur,

leading to the formation of a micro-annulus between the two surfaces. Cracks
or micro-annuli may partially or fully penetrate the length of the barrier, with
different implications for the extent to which the rate of permeation is changed.
168
28
5.3.1
5.3.2
Shrinkage and expansion
169
Shrinkage of barrier materials may occur as drying shrinkage resulting from the
evaporation of a liquid constituent of the barrier material, where it is in contact
with a gas phase. Alternatively it may occur as the result of processes occurring
during the materials ongoing solidification and hardening processes.
170
In the case of cement and similar materials, this process is referred to as

autogenous shrinkage in which water in the original slurry is incorporated
chemically into solid reaction products, leading to a reduction in volume. In the
case of thermoplastics, shrinkage will occur as the material changes from a
liquid to a solid, whilst the crosslinking processes occurring during the setting
and hardening of resin-based polymer products also lead to shrinkage. With
notable exceptions, all metals shrink as they solidify. Temperature reduction
may have a similar effect on certain materials.
171
Where shrinkage is restrained (for instance, in a permanent barrier within the

casing where the sides of the barrier are bonded to the sides of the casing)
stresses will develop in the material. In the case of viscoelastic materials, such
as polymers and gels, there is likely to be some relaxation of stress. As stress
increases, two possible modes of failure are possible:
Where the tensile strength of the bond at the barrier-casing interface is
weaker than the barrier material, de-bonding of the barrier from the casing
will occur, leading to the formation and possible growth of a micro-annulus;
Where the opposite is true, cracking of the barrier will occur.
172
Example: in order to determine the relative magnitude of flow though a microannulus, the following calculation is provided - if a laminar gas flow obeys
Darcys law, then methane flow through an open 25 m microannulus around a
plug of 100 ft inside 9-5/8 casing would result in a flow 2 m3 / day with a 1,000
psi pressure differential (all atmospheric conditions assumed). This assumes
worst-case conditions in reality cracks will be filled with water, grease,
particles and gels. Furthermore, viscosities of gases are higher at downhole
pressures. Due to these effects the actual leak rate may be several orders of
magnitude lower. Details of this equation are provided in Appendix 4.
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173
174
Expansion of the barrier is also possible, either as a result of hardening

processes, chemical reactions with substances below or above the barrier, or
as a result of an increase in temperature. Where expansion occurs within the
casing, it will have the effect of placing the barrier in compression, and the
compressive strength of the barrier material becomes important in such
circumstances. Compressive failure of the interface between the barrier and the
casing is unlikely. However, as the barrier expands, it is likely that the
restraining action of the casing will cause the barrier to undergo strain in a
direction parallel to the casing, which will cause the casing-barrier bond to be
loaded in shear. The strength of this bond in shear is often relatively weak.
5.3.3
Chemical degradation
175
Chemical degradation of a barrier material requires either a reaction between

substances within the material itself, or between substances within the material
and those entering from outside.
176
Reactions may occur in the gas phase, in solution, at a surface in contact with
either a solution or gas phase, or in the solid state.
177
It should be stressed that a chemical reaction need not be detrimental in its

effects on the performance of a barrier material, and may in some cases lead to
an improvement in properties. However, where a deterioration in properties of
the material is observed, it is likely to be the result of either a transformation to
a reaction product whose properties (in terms of strength, stiffness, solubility or
permeation characteristics) are inferior to the original material, or whose
formation leads to the development of stresses capable of causing cracking.
178
Where reactions occur between substances deriving exclusively from the

material itself, the rate of reaction may be determined by the nature of the
chemical transformation, the rate of diffusion of the substance through the
medium in which the reaction is occurring (solution, gas phase or solid), the rate
of diffusion of substances through layers of reaction products, or adsorption or
desorption of species onto and from surfaces.
179
Where reactions occur between the material and external agents, the rate of
reaction is likely to be largely controlled by the rate at which the external
species are able to move into the material, either via diffusion or carried by a
fluid moving under a pressure gradient. Thus, the requirement for a low
permeation rate discussed in Section 3.1 also plays a role in protecting the
barrier from failure.
180
Dissolution can occur where barrier material constituents or products deriving

from chemical or microbial degradation of the barrier are in contact with a liquid
in which they are soluble.
181
Where there is a small and finite volume of liquid, such as in a non-connected

pore, the soluble substance will dissolve until the liquid becomes saturated with
respect to that substance. Deterioration is only likely to become significant if the
liquid in contact with the soluble constituent has a large volume or is connected
to a larger volume of itself.
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182
183
184
185
30
In such cases, mass is lost from the material, driven either by diffusion or the
transport of liquid under a pressure gradient. The mass loss leads to an
increase in porosity and a loss in strength and stiffness. Where diffusion is the
driving force, a deteriorated front will move into the barrier at a rate controlled
by this process.
5.3.4
Creep
Materials subjected to a load may undergo both an instantaneous and delayed

deformation. This delayed strain is commonly referred to as creep. Some
materials may undergo creep over months or years. The mode of barrier failure
under creep will either be one of de-bonding of the barrier material from the
casing as a result of shear stresses at this interface, or as a result of the
formation of micro-cracks in the barrier.
5.3.5
Quality of placement
186
The quality of placement is a key functional requirement for two main reasons:
Poorly placed barriers may contain channels due to incomplete
displacement.
Poor placement technique may result in heavy contamination of the
plugging materials with the displaced fluid, which may significantly affect key
material properties.
187
Deposits, including NORM, filter cake, asphaltenes, waxes and hydrates may
be present in or around surfaces in the borehole. These should be removed in
circumstances where they could compromise the function of the permanent
barrier, although many scale types may be difficult to remove.
188
Certain materials exhibit self-healing effects, i.e. a crack or defect may repair
itself. Such healing effects normally have limitations in terms of the extent to
which the defect can be self-repaired. The properties of the material both before
and after the healing reaction will need to be tested and documented.
189
The placement technique of the material is not in the scope of this document.
Details of requirements and practices can be found in the Oil & Gas UK
Guidelines for the suspension and abandonment of wells [Ref 2].
190
The qualification of plugging material would typically include tests of:

Displacement efficiency in wells with relevant wellbore fluids. This may
include segregation (sagging) of the plugging materials components.
Sensitivity to contamination with relevant wellbore fluids (due to dilution and
dispersion) that can change key properties of barrier materials.
191
Previous tests of this type have shown that test component size can be critical.
For this reason, testing may be required at different scales, e.g. small laboratory
test, mid-scale and large-scale testing. Computer simulations may enhance the
understanding of the behaviour under varying conditions, provided the output is
validated.
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192
5.3.6
Thermal expansion differences
193
Where materials with different coefficients of thermal expansion are present, the
variation in strain produced by changes in temperature may produce sufficient
strain to cause cracking. Such effects may derive from differences in the
thermal expansion of the casing and the barrier material, or from the different
materials used in composite barriers.
194
The extent to which thermal expansion differences could cause problems is

dependent on the magnitude of temperature changes and the rate at which
temperature changes occur, with a rapid rate of change being more likely to
lead to cracking. Whilst it is unlikely that significant variations in temperature will
be encountered after abandonment, the use of barrier materials that evolve
heat during hardening or are required to be deployed at an elevated
temperature may produce such changes. Additionally, materials used in the
annulus may experience temperature cycles of greater magnitude.
195
196
5.3.7
Drilling damage
A further source of leaks can be damage caused to the surrounding formation

during the original drilling process. Leakage via cracks in the formation is not
directly a barrier material issue, but it may be the case that materials and barrier
installation techniques can be chosen such that possible leak paths through
damaged formation are sealed by the barrier.
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197
Material types
198
6.1 Definition of material types
199
The materials potentially suitable as barrier materials are listed in Table 2,

which divides materials into material types, based on their chemistry and
physical nature.
200
In the case of composite materials, assignment of material type should be for

the material acting as the matrix, unless it can be demonstrated through testing
that another constituent of the composite defines the behaviour of the material
to a greater extent.
201
Barrier configurations employing discrete multiple materials which are

interdependent in providing a seal are assigned to multiple types, but require
function testing in the envisaged configuration. Multiple barriers comprising
different materials should be tested individually.
202
Many materials can be used in a foamed condition. Where it is intended that a

barrier material is to be used in such a way, it is essential that testing is carried
out on the foamed material.
203
Potential barrier materials that are not assigned to a type are outside the scope
of these Guidelines.
204
Type
Material
Examples
Cements / ceramics
(setting)
Portland API class cement, Pozmix, slag, phosphate cements, hardening

ceramics, geopolymers
Grouts (non-setting)
Sand or clay mixtures, bentonite pellets, barite plugs, calcium carbonate

and other inert particle mixtures
Thermosetting
polymers and
composites
Resins, epoxy, polyester, vinylesters, including fibre reinforcements
Thermoplastic
polymers and
composites
Polyethylene, polypropylene, polyamide, PTFE, Peek, PPS, PVDF and

polycarbonate, including fibre reinforcements
Elastomeric
polymers and
composites
Natural rubber, neoprene, nitrile, EPDM, FKM, FFKM, silicone rubber,

polyurethane, PUE and swelling rubbers, including fibre reinforcements
Formation
Claystone, shale, salt.
Gels
polymer gels, polysaccharides, starches, silicate-based gels, clay-based

gels, diesel / clay mixtures
Glass
Metals
Steel, other alloys such as bismuth-based materials
Table 2. Material types for permanent barriers

205
206
32
6.2 Critical material properties related to potential failure modes

The performance requirements of a permanent barrier within in a given set of
operating conditions mean that it is necessary to characterize certain properties
of a prospective barrier material to ensure that it is appropriate for the
application. These properties, along with further definitions, and a discussion of
their significance in relation to the potential failure modes, are listed in Table 3.
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207
Property
Definition
Significance
Permeability
Measure of the ability of a porous material to

transmit fluids under a pressure differential.
Units = darcy.
Allows estimation of lag time between placing and breakthrough and rate of release of fluid below a given length
of barrier under a given pressure differential.
Diffusion
coefficient
Proportionality constant between the flux of a Allows estimation of lag time between placing and breaksubstance moving as a result of diffusion and through and rate of release of fluid below a given length
the gradient of concentration driving the
of barrier under a given concentration differential.
diffusion process. Units = m2s-1.
Absorption
Mass of liquid taken up by porosity within a

Provides an indication of the extent to which the barrier
material. Units = % by mass, or % by volume. will swell, from which associated stresses can be
estimated. Allows calculation of permeability.
Chemical
resistance
Indication of whether the material will

chemically react with a fluid or fluids.
Typically indicated as resistant, limited
resistant, not resistant.
Volume
change
Change in volume. Units = None (strain) or % Allows stresses resulting from expansion or shrinkage to
by volume.
be calculated.
Modulus of
elasticity
Ratio of uniaxial stress to uniaxial strain.

Units = Pa = Nm-2
Provides an indication of the extent to which the

properties of the barrier material will change
Allows calculation of magnitude of deformation of barrier

under a given pressure.
Poissons ratio Ratio of lateral to axial strain in a material

loaded uniaxially in the axial direction. No
units.
Allows calculation of lateral deformation of barrier under a

given pressure (in combination with modulus of elasticity)
Cohesion
Allows calculation of shear failure of the plug material.

Linked to tensile strength.
A strength property of granular materials that

indicates the cementation strength between
the grains under shear stress. Units = Pa =
Nm-2.
Internal friction A strength property that describes a granular

angle
materials ability to increase load-bearing
capacity (shear stress) with increasing
confinement. Units = degrees.
Allows calculation of the increased load-bearing capacity

of granular plug material with increase of the
confinement. Only strength property after significant
plastic deformation resulting in significant reduction in
UCS and loss of cohesion.
Hydrostatic
yield
Hydrostatic stress (i.e. stress applied

uniformly in all directions) at which plastic
deformation occurs. Units = Pa = Nm-2.
Indicates the onset of pore collapse in granular materials.

This failure mode is plastic and results in irreversible
deformation. Beyond this stress level the material will
gradually lose cohesion and hence load-bearing capacity.
Tensile
strength
Stress at failure under a tensile load. Units =

Pa = Nm-2.
Gives maximum tensile stress that can be withstood by

barrier.
Unconfined
compressive
strength
Axial compressive stress at which a material

fails. Units = Pa = Nm-2.
Gives maximum compressive stress that can be

withstood by barrier.
Hardness
Ability of a material to resist penetration of its

surface.
Easy quality assurance / quality control test. For certain

materials, hardness can be related to yield strength.
Shear bond
strength
Stress at which bond between two materials

fails under shear loading. Units = Pa = Nm-2.
Allows calculation of pressure differential that can be

withstood by the barrier before movement takes place.
Tensile bond
strength
Stress at which bond between two materials Gives maximum tensile stress that can be withstood at
fails under tensile loading. Units = Pa = Nm-2. the barrier casing interface.
Creep
Non-instantaneous linear deformation under

constant load with time. Units = strain rate
%/s for a given stress.
Allows prediction of ultimate dimensional change of a

barrier under a given pressure differential or other load.
Fatigue life
Number of stress cycles of a specified

character that an article can undergo prior to
failure. Units = Cycles for a given stress
range cycle.
Allows projection of longevity of barrier experiencing a

specified cyclical stress regime. In the case of materials
with an endurance limit (cyclical stress amplitude below
which failure through fatigue will not occur), allows
assessment of whether there is a risk of fatigue.
Decomposition Temperature at which barrier material begins

temperature
to thermally decompose. Units = oC (oF) at
given pressure and environment composition
Density
Mass per unit volume. Units = kg/m3.
Allows assessment of the upper operating temperature or

whether barrier will deteriorate.
Easy QA/QC test. Allows assessment of likelihood of
barrier moving as a result of imbalance between densities
of barrier and well fluids.
Table 3. Properties of barrier materials related to the potential failure modes.

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208
34
Approach to defining acceptance criteria for mass

transport properties
209
It is necessary to define certain criteria for some of the properties listed in Table
3, such that it can be demonstrated as part of a qualification that a material
being considered for use in a permanent barrier is appropriate for the
application. In the case of many materials this is based on the probable range
of service conditions and the likely characteristics of the different Material
Types. However, in the case of mass transport properties (diffusion or flow of
fluids through the permanent barrier) the approach has been taken to relate this
to the performance of cement. This philosophy is outlined below.
210
Since the permanent barrier is effectively reinstating the caprock, the

acceptance criteria are based on the performance of the caprock. Specifically,
the length and permeation characteristics (permeability or diffusion properties)
of the barrier should be such that the rate of release of fluids in the well should
be equal or lower than that of the caprock once breakthrough has occurred.
211
It should be stressed that this is a very conservative requirement, since the

cross-sectional area of a barrier will be many orders of magnitude smaller than
the area of caprock covering a reservoir. Thus, a moderately higher rate of
release per unit area through a barrier relative to the caprock is likely to make
only a small difference to the total release rate from a reservoir.
212
North Sea caprock permeability values are discussed in Appendix 5, which are
normally better than can be achieved with standard cements the permeability
of good cement is typically below 10 microdarcy. However, industry experience
has found that 30 m (100 ft) cement barriers perform to a level which has been
satisfactory within the historical timeframe of commercial oil and gas production.
213
Example: The Oil & Gas UK Guidelines for the suspension and abandonment
of wells [Ref 2] require 30.5 m (100 ft) of good cement. Using a permeability
value typical for good cement (20 microdarcy) and a pressure differential of
6.9 MN/m2 (1,000 psi), a release rate of 0.25 m3 of gas per year would be
obtained for this length of barrier in a 7 casing, assuming the absence of
cracks or micro-annuli. Details of this calculation are given in Appendix 6.
214
Therefore, it is deemed appropriate that the performance criteria for mass

transport through permanent barrier materials should be equivalent to that of
good cement.
215
As discussed above, it is proposed that an appropriate maximum permeability

of 20 microdarcy as the acceptance criteria for the qualification of a cement
barrier of the sort discussed above. An equivalent diffusion coefficient would be
around 4x10-8 m2/s (30.5 m (100 ft) length, 7 casing, partial pressure of
methane of 34.5 MPa (5,000 psi)). Details of this calculation are given Appendix
7. The pressure value used is appropriate for a shallow North Sea well.
Alternative pressure values for different well types can be obtained from
Table 1.
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216
However, it is recognised that different materials may have different

permeabilities or diffusion coefficients, which will influence how they are
employed. Where permeability is lower, a shorter barrier may be installed, and
greater barrier lengths could be used for more permeable materials. Therefore,
it is proposed that the performance criteria for mass transport is the theoretical
release rate of methane from the top of the barrier (once a steady state has
been reached) for the intended barrier configuration and anticipated service
conditions. The calculation methods described in Appendices 6 and 7 should be
used to estimate this release rate value using permeability or diffusion
coefficient values obtained from characterisation of the material.
217
Permeabilities and, in some cases, diffusion coefficients will be measured using

fluids other than methane, and will differ somewhat from those of this gas.
However, given the uncertainties associated with predicting long-term
performance, this approach will at least provide an appropriate indication of
performance.
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218
Experimental work plan
219
The following section outlines the types of test that may be required for
qualifying a barrier material. Not all tests are appropriate for all materials Section 9 identifies the tests which are most appropriate for each of the material
types identified in Section 6 based on their likely failure modes.
220
All testing programmes should include both a function test and a programme of
ageing testing, as outlined below. The involvement of a qualified third party
witness (independent competent body) will increase credibility of the test results
with customers and the regulator.
221
222
223
8.1 Literature investigation

A mandatory literature search should be conducted to determine critical
material properties. It must also include exploration of the likely mode of fluid
permeation, failure modes of the material in question, its chemical functional
envelope and changes to properties which will occur at elevated temperatures.
This is to be documented as part of the qualification of the barrier material.
8.2 Permeation testing
224
The transport of fluids through barriers can be via flow or diffusion. When
evaluating the sealing ability of a barrier material, it is necessary to select the
most relevant type of mass transport to be measured. Where porosity is absent,
diffusion is likely to be the main mass transport mechanism. In the case of
porous materials, mass transport will occur via both flow and diffusion.
However, for the pressure gradients encountered across a barrier under typical
North Sea conditions, the flux of fluid resulting from flow will normally exceed
that resulting from diffusion by more than one order of magnitude. Therefore,
permeability measurements are of primary relevance for porous materials.
225
In the case of both permeability and diffusion measurements, an accuracy

within 50% of the true value is required.
226
36
8.2.1
Permeability
227
Permeability is usually measured in porous materials using either water or air

as the flowing medium. Some of these test methods are discussed below.
228
A key issue for permeability measurements is ensuring fluid is not able to divert
around the specimen. Water permeability measuring techniques achieve this in
various ways, including encapsulating the sides in bitumen or resin [Ref 10, 12]
or by confining the sides within a pressurised sleeve [Ref 12] or triaxial cell.
This last approach is adopted in the Hassler cell, which was developed for the
oil and gas industry for the measurement of rock permeability. The technique
also uses a chromatography pump to maintain a constant pressure.
229
Liquids used for testing need not be limited to water, and previous research
using such equipment has used both oil and brine [Ref 13, 14].
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230
In the case of non-setting grout-type barrier materials, if the pressure difference

exceeds the shear strength of the grout, the permeability value obtained will be
unrepresentatively high. In such cases, the shear strength of the material must
be determined such that a suitable pressure difference, or set of pressure
differences, may be selected for testing.
231
An alternative approach to measuring permeability is to use the decay of a pore

pressure pulse applied to one side of a specimen saturated with a fluid held in a
triaxial cell and measured on the opposite side [Ref 15]. The magnitude of
decay can then be used to infer the permeability of the material.
232
Gas permeability measurement can use similar apparatus to water permeability

measurement, although different configurations of pumps and flow
measurement devices are required. Success has been obtained by using very
similar apparatus to the Hassler cell with air [Ref 16]. Steady-state conditions
are achieved in a much shorter time. However, specimens must be dried prior
to testing, and this is considered unacceptable due to the changes it is likely to
induce in many materials. Thus, water permeability measurements on saturated
specimens at 20oC are required under the experimental workplans proposed in
this document. However, where possible, translation to gas permeability values
should be carried out. Such translation should take into account gas slippage,
sometimes referred to as the Klinkenberg effect, where a layer of gas molecules
is present at pore walls whose behaviour differs from that of the molecules in
the rest of the porosity.
233
It should be noted that before a non-wetting fluid (such as a mixture of

hydrocarbons) can enter a water-saturated porous barrier, the pressure acting
on the barrier surface must exceed the capillary entry pressure, pce. This
pressure is required to overcome the difference in pressure between the fluid
on the outside of the barrier and the water within the pores. The capillary entry
pressure is described by the equation:
234
Where:
235
the pore radius (m);
the surface tension of water (N/m); and
the contact angle of the water with the pore surface.
Capillary entry pressure must only be exceeded when the contact angle
between the barrier material and water is >90. Whilst the capillary entry
pressure could potentially be exploited as a means of resisting permeation of
the barrier by fluids, the contact angle and pore radii are prone to modification
with time, and the approach taken in this document is to discount this
phenomenon in terms of material qualification.
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236
237
238
239
Diffusion
Diffusion testing is normally conducted using a configuration in which two

chambers are separated by a specimen of the material under investigation. The
first chamber is a reservoir filled with the fluid or chemical species of interest, or
a mixture containing the substance of interest, whilst the second is filled with a
reservoir containing a fluid in which the substance of interest is absent. The
concentration of substance is measured in the second chamber. Once steady
state diffusion is achieved, the diffusion coefficient can be obtained using the
change in concentration with time.
8.3 Interaction with fluid

8.3.1
Absorption
240
Absorption of fluid (water, liquid hydrocarbons, methane, CO2 etc.) by a solid or

gel will lead to expansion. Measurement of absorption can therefore give an
indication of the extent to which swelling will occur, if the characteristic
behaviour of the material is already known. Identification and measurement of
absorption is best addressed during ageing testing (see Section 9.10), during
which the material is in contact with fluid. Through mass measurements,
absorption can be identified as a gain in mass.
241
In the case of gels, the amount of absorption is expressed in terms of an

absorption index, which is the ratio of the mass of gel over the original mass of
dry solids used to form the gel. This parameter may provide a useful indication
of the extent to which the nature of the gel has changed after ageing.
242
38
8.2.2
8.3.2
Leaching, corrosion and chemical resistance
243
The leaching or corrosion of a barrier material (or constituents of the barrier

material) are likely to lead to changes in critical properties, including most
mechanical properties and permeation characteristics. As with absorption, mass
measurements before and after ageing testing are essential to assess the
magnitude of leaching, with leaching indicated by a loss in mass.
244
It should be stressed that where absorption and leaching occur simultaneously,

the magnitude of mass change will be limited by opposing movements in mass
into and out of the material, possibly giving the impression of acceptable
behaviour when this is not the case. However, it is likely that other
characteristics measured after ageing (e.g. mechanical and permeation
properties) would nonetheless highlight problems with leaching. Moreover a
measurement of the change in dry mass of a barrier material specimen after
ageing will confirm whether mass loss due to leaching has occurred (see
Section 8.10).
245
Chemical reactions between fluids and the barrier material may also produce
changes in properties which may be detrimental. Chemical reaction may not
involve a loss in mass, and may involve an increase in mass, meaning that
mass change measurements are unlikely to be useful in assessing chemical
resistance. Furthermore, degradation mechanisms such as chain scission of
polymers by hydrolysis may involve minimal change in mass. However, as for
leaching and corrosion, it is likely that a lack of chemical resistance will be
identified through testing after ageing (see Section 8.10).
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246
It is also important to establish through appropriate testing the possibility of

reactions between the casing steel and the barrier material. For instance, a
metal barrier delivered in molten form can potentially produce a phenomenon
known as liquid metal embrittlement where contact with the molten metal
produces a weakening of the steel.
247
Assessment of barrier material degradation due to exposure to gamma

radiation from caprock or NORM scale may be necessary.
248
Visual inspection is required with documentation of observed deterioration

supported by photographic evidence. Retention of samples is a good practice.
249
All metallic barrier materials must conform to ISO 1516 / NACE MR0175 with
respect to their resistance to corrosion in H2S-bearing environments.
250
251
8.4 Dimensional stability

8.4.1
Expansion / swelling
252
Expansion of barrier materials can be divided into two forms that which occurs
during the hardening of a material which is initially in a liquid or granular form,
and that which results in expansion in the hardened state, possibly (but not
exclusively) as the result of absorption of fluid.
253
Expansion may be measured using a range of techniques depending on the

material. In the case of cement, the annular ring method described in ISO
10426-5 is appropriate, and is likely to be applicable to other materials.
Alternatively, a pump connected to an ultrasonic cement analyser (UCA) may
be used for volume change with cement-type material.
254
Swelling of rock in general is covered by the ISRM suggested method:

Determination of the swelling strain developed in an unconfined rock specimen.
Additionally, given the configuration of permanent barriers within the casing, the
method Suggested method for determination of the swelling strain index for a
radially confined specimen with axial surcharge is also potentially useful.
255
Measurement of swelling in rocks prone to expansion on a significant scale is

covered by the ISRM suggested methods, Laboratory testing of argillaceous
swelling rock, and Laboratory testing of swelling rocks - Part 3 - Determining
axial and radial free swelling strain. These methods may be applicable to other
materials in some cases.
256
Barrier expansion within the casing may not be detrimental for some materials,
since it will increase the friction between the barrier and the casing. However,
where materials are brittle and elastic, excessive expansion may cause damage
to both the barrier and the casing-barrier interface.
257
Visual inspection is recommended with documentation of observed

deterioration supported by photographic evidence. Retention of samples is a
good practice.
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258
8.4.2
Shrinkage
259
As with expansion, it is helpful to subdivide shrinkage into that occurring during

and after hardening, where applicable, since the effects have different
implications.
260
In general, shrinkage after hardening is more likely to have a detrimental effect

on barrier performance. This is because the stiffness of the material will be
higher and thus stress levels resulting from restrained shrinkage will be higher.
261
In some cases, this shrinkage can be measured using identical techniques to

those used for expansion, such as the ISO 10426-5 ring test for cement. The
shrinkage of clays and clay-like materials is covered by ASTM D4943.
262
A range of ISO test methods are available for different types of polymer. For
instance, ISO 2577 deals with thermosetting polymers.
263
Where materials undergo a rapid drop in temperature, there exists the risk of
thermal shock, where the corresponding drop in volume occurs to different
extents in different parts of a materials volume. This can lead to the
development of stresses which produce mechanical failure. It is likely that the
large drop in temperature required for thermal shock to occur, makes materials
which would be placed in a molten state to be the main candidates glass,
thermoplastic polymers and metals. It is probable that glass would be most
prone to such a mechanism of failure, although where such a method of
placement is employed, this matter would need to be investigated as part of the
work plan.
264
8.4.3
Differential thermal expansion
265
The coefficient of thermal expansion can be measured using the technique

described in ASTM E228. This technique uses a dilatometer to determine linear
expansion over a range of temperatures.
266
The appropriateness of using two materials in contact with each other (barrier
casing, barrier formation etc. can be judged by estimating the likely
temperature range experienced by the materials once the barrier is in position
(including during deployment and hardening processes) and calculating the
difference in strain displayed by each material over this range, using the
equation:
267
Where:
268
40
the strain difference;
T =
the temperature range (K);
the mean coefficient

over T (K-1).
of
thermal
expansion
of
material
In certain cases, for instance where the properties of steel used in a casing are
well documented, coefficient of thermal expansion values from the literature
may be used.
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269
8.4.4
Creep and stress relaxation
270
Long-term deformation as a result of creep can occur in tension or

compression. Typically, creep in compression is observed in porous materials.
271
The method described in ASTM C512-10 is suitable for the measurement of

compressive creep in cement and other brittle elastic materials.
272
Creep in tension is the main concern for polymers and metals. In the case of
polymers, creep testing is covered by ISO 899-1, whilst ISO 204 covers metals.
273
Elastomers may undergo permanent deformation when subject to a long-term

compressive load. This form of creep is known as compression set or stress
relaxation, and a method for its measurement is described in ASTM D395. The
capacity for elastomers to undergo stress relaxation may be problematic in
cases where expansive elastomers are used to create a sealing stress between
a barrier and the casing, since it will lead to a reduction in this stress.
274
For most materials employed in abandonment, creep is undesirable. However,

a strategy may be employed to exploit the formation in which the well is located
such that, over longer periods of time, it undergoes creep to such an extent that
it seals the well, thus ultimately rendering the permanent barrier redundant. In
such cases, a high creep rate is desirable.
275
Creep testing
abandonment.
276
should
be
conducted
using
expected
stresses
after
8.5 Mechanical testing
277
The objective of mechanical testing of barrier materials is to establish a yield

surface for the material. The yield surface defines the elastic region of the
materials response to stress. Outside the yield surface the material will lose
some of its load-bearing capacity and, depending on the material, may start
fracturing. For certain materials (e.g. cement, brittle polymers), it is desirable
that barrier material operates exclusively within the elastic region. The testing
procedure will also produce engineering design parameters that can be used in
engineering calculations towards achieving this (modulus of elasticity, Poissons
ratio, cohesion, unconfined compressive strength (UCS), internal friction angle
etc). In the case of ductile materials, operating in the elastic region may not be
necessary or even desirable.
278
Deformation and strength properties of most materials are dependent on both

temperature and the chemical environment with which they are in contact.
Therefore, mechanical testing should be performed at the expected operational
temperature and in the expected chemical environment.
279
The following tests are potentially useful for characterising the material:
triaxial testing, with determination of elastic modulus, cohesion, internal
friction angle and Poissons ratio;
hydrostatic compression testing;
UCS determination; and
tensile strength determination.
280
These tests are discussed in further detail below.
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281
Triaxial testing
282
Many materials that are candidates for use in permanent barrier applications
can be characterised using triaxial testing, in accordance with the methodology
described in the ISRM Suggested method for determining the strength of rock
materials in triaxial compression. The method uses cylindrical specimens
whose length is equal to, or longer than, twice the diameter to avoid end effects.
Correction for other shapes / size is required, as detailed in the ISRM
suggested method.
283
Triaxial testing is conducted using a triaxial cell capable of applying a confining

stress around the circumference of the cylindrical specimen and an axial stress
at the top and bottom of it. There must be a means of accurately measuring
axial and radial deformation during testing.
284
Measurement of elastic modulus, cohesion, internal friction angle and Poissons

ratio is possible using this method.
285
8.5.2
Elastic modulus
286
The elastic modulus of a material provides a measure of the strain a material

experiences under a given stress whilst it is operating within the elastic
deformation region.
287
Static elastic modulus measurements can be obtained from triaxial testing,

although they can also be obtained via other means. ASTM C469 can be used
for cements and similar materials, whilst ISO 3312 is appropriate for metals.
Additionally, analysis of stress strain-curves obtained from tensile or
compressive testing can be used to obtain the elastic modulus, such as
described in ISO 527-1 for polymers.
288
Measurement of dynamic elastic modulus can be obtained from acoustic

velocities. This Poissons Ratio is called the dynamic Poissons Ratio. This
value will differ from that obtained from triaxial testing, referred to as the static
Poissons ratio. Static elastic properties should be used for engineering
calculations. An example of such a method is ASTM E1876, for metals.
289
290
291
292
42
8.5.1
8.5.3
Cohesion
Cohesion is a strength property of granular materials that indicates the

cementation strength between the grains under shear stress. Cohesion can be
found from at least three triaxial tests at three different confining pressures.
8.5.4
Internal friction angle
The internal friction angle is a strength property that describes a granular

materials ability to increase load bearing capacity (shear stress) with increasing
confinement. The internal friction angle can be found from a minimum of three
triaxial tests with three different confining pressures. The internal friction angle
can be derived from the slope of the failure line in a Mohr-Coulomb diagram.
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293
8.5.5
Poissons ratio
294
The Poisson's Ratio provides a measure of how much a material expands or

contracts in the direction perpendicular to the direction of an increase in
compressive or tensile load respectively. If the material is confined, the
Poisson's Ratio provides a means of calculating the increase in stress in the
direction perpendicular to the direction of an increase in load of the material.
295
The Poisson's Ratio is found from triaxial tests of materials where both axial
and radial deformation of the material is measured.
296
The Poisson's Ratio can, as is the case with all elastic properties, be calculated
from acoustic velocities. This Poisson's Ratio is called the dynamic Poisson's
Ratio. This will not be the same Poisson's Ratio as the one derived from triaxial
testing, referred to as the static Poisson's Ratio. Static elastic properties
should be used for engineering calculations. An example of such a method is
ASTM E1876, for metals.
297
298
299
8.5.6
Hydrostatic compression testing
Hydrostatic compression testing can also be performed within a triaxial cell by

increasing the confining and axial stress on the specimen simultaneously and
uniformly. The test should be continued beyond the point where the material
yields hydrostatically, thus allowing the hydrostatic yield point to be determined.
8.5.7
Unconfined compressive strength (UCS)
300
Unconfined compressive testing is typically carried out to failure on either

cylinder or cube specimens. Unconfined compression testing is likely to be most
useful in the case of brittle elastic materials such as cement. For cement,
testing is covered by ISO 10426-2. This method may not be suitable for highly
elastic materials.
301
A method for unconfined compressive strength measurement of rock is

described in the ISRM suggested method, Suggested method for determining
the uniaxial compressive strength and deformability of rock materials.
302
Methods for the compressive strength testing of metals are described in ASTM
E9.
303
8.5.8
Tensile strength
304
Where a barrier material is brittle and elastic, tensile strength should be

determined using a splitting (Brazilian) test (ASTM C 496).
305
Tensile strength of ductile materials should be tested using dogs bone type
specimens in accordance with standard methods. Testing of polymers is
covered by ISO 527-1 and 527-2, whilst ISO 6892-1 is appropriate for metals.
306
307
8.5.9
Hardness
In most instances, hardness would not necessarily be a characteristic

specifically required by a barrier material. However, hardness measurements
can be related to yield strength for many materials, and may also provide an
indication of deterioration when conducted before and after ageing testing.
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308
Hardness testing can be carried out in a number of ways. Hardness of polymers

is normally measured using a shore durometer test (ISO 868) which measures
the depth of indentation of a hardened steel rod in a polymer surface using a
standard applied force.
309
The hardness of metal may be measured by several methods including the

Rockwell test (ASTM E18), which measures the depth of penetration of an
indenter, firstly after a minor load is applied, and then after a larger load. The
Brinell and Vickers tests (ASTM E10 and ASTM E384 respectively) both also
use indenters, although hardness is measured from the diameter of the
resulting indentation.
310
The hardness of brittle materials is best determined using the Knoop test
(ASTM E384) which also uses the diameter of an indentation left by an indenter
as the measure of hardness.
311
For rock from formations and rock-like materials, ISRM suggested methods
exist for Shore hardness, indentation hardness and rebound hammer
measurements.
312
313
314
44
8.6 Bond strength

The bond between a barrier material and the casing can fail through two
different mechanisms. Firstly, a pressure differential across the barrier could
potentially lead to a shear failure of any bond between the barrier and the
casing and / or movement of the barrier. Secondly, shrinkage of the barrier
material may place sufficient tensile stresses on any bond between the barrier
and the casing to cause failure at this interface.
8.6.1
Shear bond strength
315
The shear bond strength provides an indication of the pressure differential

required for a barrier to be moved from its position and, in the case of materials
where a physical bond exists between the casing and the barrier, the shear
stress required for debonding to occur.
316
Whilst no standards exist for such measurements, the value can be determined
by casting material inside a length of steel pipe and measuring the force
needed to push it out.
317
Since bond strength measurements will be partly dependent on the substrate

used and its rugosity, both should be documented. Rugosity can be measured
using the technique described in ASTM D7127.
318
Whilst there is no bond between non-setting grouts and the casing, there exists
the possibility that pressures below a barrier of this type will be sufficient to
extrude it from the casing. It is therefore recommended that a laboratorybased assessment of extrusion pressure be conducted for such materials.
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319
320
321
322
323
324
325
8.6.2
Tensile bond strength
Whilst a possible failure mechanism is the debonding of the barrier from the
casing under tensile loading, the absence of standards for the measurement of
tensile bond strength and the extreme sensitivity of this property to surface
condition renders its meaningful characterisation impossible. Thus, at the
present time, there is no requirement for tensile bond strength measurement.
8.7 Fatigue life

Cyclical loading of many materials may lead to failure through fatigue. Fatigue
is generally not applicable for permanent barrier materials, but may be relevant
for particular circumstances, e.g. for gas storage wells cycling. In this case, it
will require testing as part of the material qualification.
8.8 Decomposition temperature

As materials are exposed to increasingly high temperatures, they will undergo
changes of state and chemistry which will alter their mechanical behaviour. In
certain cases materials will undergo thermal deterioration (via pyrolysis and
thermolysis) leading to complete or partial destruction of the material. In the
case of certain potential barrier materials it is recommended that they are
analysed using either thermogravimetric analysis (TGA), differential thermal
analysis (DTA) or differential scanning calorimetry (DSC) to establish whether
the material undergoes any changes at temperatures close to the likely
operating range. Where this is found to be the case, further investigation of the
nature and likely consequences of the change is required.
8.9 Density
326
The density of a barrier material can be used as a simple quality assurance or

quality control test following the fabrication of test specimens. However, it is
also a useful means of establishing whether leaching has occurred during
ageing testing. Furthermore, it can provide useful values for calculations to
establish the likelihood of barrier movement resulting from differences between
barrier density and fluid densities.
327
Density can be measured using a number of techniques, but the most common
technique involves weighing the specimen in air and in water. Density
measurement for hardened cement and similar materials is best addressed
using the methods described in ASTM C138. Polymers are covered by ISO
1183-1. Metals are covered by ISO 3369. The measurement of rock density is
described in the ISRM suggested method, Determining Water Content,
Porosity, Density, Absorption and Related Properties.
328
The density of non-setting grouts can be measured using a pressurized mud

balance following the method described in ISO 10426-2.
329
Localised changes in density can be observed non-destructively within test

specimens using techniques such as X-ray computed tomography (CT) and
magnetic resonance imaging (MRI).
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330
46
8.10 Ageing testing
331
Ageing testing involves exposing materials to likely worst-case downhole

conditions, periodically measuring changes in selected properties, and
employing extrapolation techniques to establish likely rates of deterioration over
longer timescales. For some materials, temperatures in excess of those
encountered in reality may be used to achieve accelerated ageing during the
testing programme, which can provide further useful data for the extrapolation
process. It should be stressed that changes in material properties over time can
potentially be either detrimental or beneficial.
332
Only certain material properties will provide a useful indication of likely rates of
deterioration. These have been selected for different material types in Section
10. The ageing process should be achieved by storing specimens in an
autoclave at a pressure and temperature which reflect the worst-case downhole
conditions, in contact with simulated in situ fluids (SIFs) whose composition has
been formulated to reflect those both above and below the barrier. Specimens
should be saturated with the SIF prior to placing in the autoclave.
333
Endeavours should be made to use an autoclave configuration which

maximises the ratio of SIF to material. This ratio should be documented. Where
the ratio of fluid to material is less than the real situation, the results of ageing
should be viewed as merely indicative. It should be stressed that the autoclave
environment is likely to be more aggressive than many of the environments
encountered by barrier materials in situ, since in the real situation much of the
fluid will be present within porous media in contact with the barrier, and
availability of aggressive substances will thus be limited. The contact area
between the material and the fluid is therefore significantly larger in the
laboratory than in a real situation. In the laboratory test the chemical reaction
itself will be the rate determining step, whereas downhole, this will be the
diffusion of reactants and products to and from the interface. The reaction will,
thus, initially be faster in the laboratory than it would be downhole.
334
It is suggested that specimens are removed for testing after ageing periods of
three, six and twelve months. An individual autoclave should be used for
measuring the ageing behaviour of each material characteristic, with three
specimen duplicates for each measurement. Furthermore, an individual
autoclave should be used for each ageing period used.
335
The autoclave should be wholly resistant to the chemical environment required.
336
A literature investigation is highly recommended in the preparation of the ageing

testing plan.
337
Specimens should be removed from the autoclave at ages of one, three, six
and twelve months for testing, or longer. Properties measured after ageing will
depend on the material, but would typically include tensile strength, mass,
volume, visual appearance, chemical condition (e.g. X-ray diffraction, infrared
spectroscopy, SEM) and permeability. Analysis for cracks using microscopy,
ultrasound, NMR, or acoustic emission may also be conducted.
338
The ageing process must be carried out in an appropriate manner so as to

avoid damage to specimens during compression and decompression. Samples
should be saturated in the autoclave before the aging conditions are
established, until a mass change of <0.1 % is observed over a 24 hour period.
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339
During decompression, pressure reduction must follow an agreed rate to avoid

gas generation and damage to the specimen. For cement, the API specifies
0.7 bars / minute (10 psi / minute). It is recommended that this rate is
determined for the specific material and gas. It should be noted that the most
appropriate rate could potentially be variable.
340
For polymers and composites, to reduce the potential of decompression

damage, the pressure should ideally be released as slowly as possible over
weeks. However, for practical reasons the following procedure is
recommended:
If the test pressure is higher than 100 bars (1,450 psi), reduce pressure to a
minimum of 100 bar at an average rate of 0.5 bar / minute (7 psi / minute)
and leave the system at temperature for 24 hours;
Cool to ambient temperature;
Reduce remaining pressure at an average rate of less than 0.5 bar / minute
and the leave test specimens undisturbed until the next day.
341
Testing with H2S and methane at high pressure presents potential health and
safety issues, which must be appropriately addressed.
342
Further information on procedures and conditions for ageing testing can be

found for thermoplastics in ISO 2578, for elastomers in Norsok M-710 and for
thermosetting polymers in EN 13121-2.
343
Once a series of measured values are obtained for the full sequence of ages, a
procedure for extrapolation to the required barrier lifetime can be followed. An
example of such a procedure is shown in Figure 8, where extrapolation has
been conducted on a deteriorating material property. The uncertainty
surrounding such an extrapolation means that the lower 95% confidence limit is
used as the prediction of deterioration in performance. It should be stressed
that caution should be employed when interpreting extrapolated results of this
type, and such results should be viewed, at best, as being indicative.
344
For certain materials (in particular, polymers) exposure to elevated

temperatures has the effect of accelerating the ageing process. Temperatureaccelerated ageing may be applied as long as it can be demonstrated that such
an approach is valid for the material being evaluated, and the temperature
employed is below the decomposition temperature of the material. In the case
of polymers, extrapolation in line with the methodology described in ISO 2578
may be conducted. This approach is outlined in Figure 9, where a series of
temperatures are selected for ageing testing (inset 1), testing to a failure point is
conducted at each temperature (inset 2), and the time to failure for each testing
regime is then extrapolated to the envisaged operating temperature on a plot of
the reciprocal of absolute temperature (1/T) versus the natural log of the time to
failure (ln t) to obtain a prediction of the materials lifetime (inset 3).
345
Where lifetime expectancy calculations are presented only recognised and

appropriate extrapolation techniques should be used. The methodology and
underlying assumptions must be clearly presented.
346
The use of elevated temperatures to produce accelerated ageing is not suitable

for Portland cement and should be assumed to be unsuitable for other materials
unless evidence proving otherwise is available.
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347
In the case of polymer degradation, where sufficient data is available in the

literature, it may be possible to employ the Arrhenius rate law to predict the rate
of degradation at a given service temperature, thus allowing screening of
unsuitable materials. The law is described by the equation:
348
Where:
a
the degree of degradation;
time (s);
a pre-exponential factor;
Ea
the energy of activation (J/mol);
is the gas constant (J/molK);
temperature (oK); and
f(a) =
349
a function describing the dependence of the rate of degradation on the

degree of degradation (s-1).
Values of A and Ea may be available in the literature, along with descriptions of

f(a).
PROPERTY, (%)
350
TIME, (years)
Figure 8. Deterioration of a material undergoing ageing testing, with
extrapolation to future ages (dashed line). The dotted lines are the 95%
confidence limits of the extrapolated line.
48
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351
Figure 9. Procedure for predicting the lifetime of a material using a series of

ageing tests conducted at a series of temperatures.
352
8.11 Function test
353
A function test is required to demonstrate that the material can perform a

sealing function at a rated pressure in a well bore. This is to be done using an
at-surface test configuration, as shown in Figure 10. The test follows the
principles of ISO 14310 without temperature cycling.
354
For the function test, a 7 casing joint will be erected at an angle of 45 to be

filled with a test barrier comprising 30 ft of the potential permanent barrier
material. The casing joint should be steel and have a weight between 43 and
52 kg/m (29 and 35 lb/ft) compliant with the required pressure rating. The
construction will comply with regulations regarding pressure vessels. There will
be a gas / water injection nipple at the bottom and a pressure recording at the
top. There will be further pressure recordings made along the casing, such that
extrapolation of measurements can be used to establish the pressure rating of a
longer plug. The pressure measurement will, as a minimum, be taken at the
high-side of the casing. Other instrumentation may be added to assist in
validating calculations and modelling.
355
Prior to filling, the roughness rugosity - of the inner surface of the casing
joint should be characterised in accordance with the method described in ISO
11960. The results of surface roughness characterisation should be
documented.
356
Before placement of the material, the casing is heated to a specified

temperature (+/- 5 C) that simulates the anticipated downhole conditions. This
temperature is normally maintained during the entire duration of the functional
test. The actual temperature is to be documented. To suit particular operating
conditions, another qualification temperature can be chosen.
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357
Before applying the load, the product must have reached a stable condition, i.e.
has set, been cured, developed full strength, and is fully bonded to the casing.
358
A test with water will be used for the first test sequence. The water pressure
selected will be the expected hydrostatic pressure in the envisaged application.
Nitrogen will be used for a second test sequence; this is intended to simulate
methane gas. The gas pressure used should reflect the likely reservoir
pressure. The water or gas pressure will be increased in 10 steps to the rated
pressure over a period of 10 hours. An observation period should exceed three
days.
359
Where pressure and temperature fluctuations are anticipated subsequent to

abandonment, it may be appropriate to include an evaluation of barrier material
performance under the anticipated fluctuating conditions.
360
A log of all activities with a timeline is to be documented.
361
The test conditions which should be specified are the test pressure rating, the
maximum and minimum temperature, whether the material should be filled with
brine, water or oil prior to testing, and what test fluids are to be used (nitrogen,
water etc). The results of the test should be reported in terms of whether the
test barrier withstood the test pressure for at least 3 days, the pressure profile
through the length of the barrier, and the rate of flow through the barrier, if any.
362
If the material to be characterised evolves heat during or after placement is

conducted, or requires heating during placement, instrumentation should be
included to permit monitoring of barrier temperatures. The maximum
temperature reached and the duration of elevated temperature should be
documented. With respect to heat evolution, adequate consideration must be
given to the effects of scaleup, to allow for differences in temperatures attained
by a real barrier relative to experimental results, and the consequent differences
in expansion and possible deterioration processes.
363
Gas/water receiving point

with dummy plug
during product placement
Pressure recording on high
side to allow extrapolation of
plug length. Recording points
1,2,3 are compulsory,
and 4,5, others are optional
Gas/water
injection point
with dummy plug
during product
placement
Accommodates 30 ft product
7 casing, instrumented
with spaced pressure gauges.
45 degrees inclination.
4
2
Product overflow port
with disposable valve
5
1
Product fill port with disposable valve
Figure 10. Configuration for a functional test.
50
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364
8.12 Field trial
365
Whilst laboratory testing of potential barrier materials will provide evidence of

fitness for purpose and data which will assist the engineer, there is a strong
argument for ensuring that theoretical suitability is confirmed in the field. Field
trials also permit confirmation of compatibility of the barrier material with its
intended environment and an evaluation of the feasibility of scale-up from
laboratory scale.
366
Thus, where possible, it is recommended that field trial application of a given

barrier material and its installation technique are conducted. The evaluation
process should involve in situ testing and verification of the barrier, including
assessment of the extent to which contamination of the material occurs during
installation, the effect of varying loads and other external influences. Long-term
monitoring through the incorporation of instrumentation such as acoustic
transducers may also permit evaluation of any deterioration with time. The
verification method(s) and results should be documented.
367
Placement techniques should be modelled and validated.
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368
Material types specific experimental work plans
369
The following section identifies appropriate work plans for qualification testing,
based on the most likely failure modes for each material type. It should be
stressed that the suggested work plans for each material type, are based on the
typical behaviour of such materials, and that other tests may need to be
included to address non-typical material characteristics. It should also be noted
that the naming of specific products in this section is not an endorsement, but is
simply used to assist readers in identifying material types. Where the results of
an experimental work plan identify a material as appropriate for use as a barrier
material, this must be followed by a function test, as described in Section 8.11.
370
For each property a requirement classification (1 to 3) is provided where:

1 = mandatory;
2 = recommended;
3 = not applicable.
371
372
52
A property requirement classified as mandatory will, in most cases, include

acceptance criteria which the material must satisfy. A property requirement
classified as recommended indicates a characteristic whose measurement is
likely to provide a useful indication of performance or provide data useful for
design purposes. Thus, in most cases, acceptance criteria are not specified for
recommended tests.
9.1 Type A: Cements, ceramics (setting)
373
This class comprises cements, including phosphate cements, ceramics,

geopolymers and salt backfill. It also includes mixtures of cement and additives
like silica, inorganic expanding agents, polymeric inclusions, permeability
reducers and density modifiers.
374
Decompression damage to specimens during ageing testing is a potential risk.

Appropriate decompression techniques should be employed.
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375
PROPERTY
REQUIRE
-MENT
ACCEPTANCE CRITERIA
AGEING
REQUIRED?
TEST
Before Ageing
After
Ageing
PERMEATION TESTING
Water permeability
See Section 8.2.1
Yes
See Section 7.
Calculated release rate
(Appendix 6)
<50%
increase
<0.25 m3/year
Diffusion coefficient
Dry mass
Measurement of mass
after drying to constant
mass at 105 oC (221 oF)
Yes
<3% loss
Absorption
During hardening
ISO 10426-5 ring test
No
<1.0% by volume
Hardened
Yes
<1.0% by
volume
During hardening
No
<1.0% by volume
Hardened
Yes
<1.0% by
volume
Differential thermal
expansion
ASTM E228
No
<1% linear strain

difference
Creep
ASTM C512 - 10
No
<1% linear strain
Triaxial Testing
Cohesion
Poissons ratio
Hydrostatic compressive
yield
UCS
ISO 10426-2
Yes
>1.4 MPa (200 psi)
>1.4 MPa
Tensile strength
ASTM C 496
Yes
>1 MPa (145 psi)
>1 MPa
(145 psi)
Elastic modulus
ASTM C469
Yes
Hardness
ASTM E384
Yes
Shear bond
strength
See Section 8.6
Yes
>1 MPa (145 psi)*
>1 MPa (145

psi)*
Tensile bond
strength
Fatigue life
Decomposition temperature
Density
ASTM C138
Yes
Stress relaxation
INTERACTION WITH FLUID
DIMENSIONAL STABILITY
Expansion / Swelling
Shrinkage
MECHANICAL TESTING
(200 psi)
OTHER CHARACTERISTICS
Bond Strength
*Minimum shear bond strength limit has been arrived at based on a calculation detailed in Appendix 10.
Table 4. Experimental work plan for Type A materials.
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376
54
9.2 Type B: Grouts (non-setting)
377
Non-setting grouts include inert particle mixtures such as sand mixtures, clay
mixtures, bentonite pellets, barite plugs and calcium carbonate. Lost circulation
pills, whilst potentially falling within this category, are excluded.
378
Certain grouts rely on gel-forming properties. When qualifying materials of this

type, evaluation of whether the material best fits Type B or Type G is required.
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379
PROPERTY
REQUIRE
-MENT
AGEING
REQUIRED?
TEST
ACCEPTANCE CRITERIA
Before Ageing
After Ageing
PERMEATION TESTING
Water permeability
See Section 8.2.1
Yes
See Section 7.
Calculated release
rate (Appendix 6)
<0.25 m3/year
<50% increase
Measurement of
mass after drying
to constant mass
at 105 oC
Yes
<3% loss

Dry mass
(221 oF)
Absorption
During hardening
Hardened
During hardening
Hardened
ASTM D4943
No
<0.4% by volume
ASTM E228
No
<1% linear strain

difference
Creep
Triaxial Testing
Cohesion
Poissons ratio
Shrinkage
MECHANICAL TESTING
Hydrostatic compressive yield
UCS
Tensile strength
Elastic modulus
Hardness
Shear bond
See Section 8.6.

Substrate
rugosity should
be measured
using ASTM
D7172.
Tensile bond
strength
Fatigue life
Density
Pressurized mud
balance
Stress relaxation
Bond Strength
strength
Table 5. Experimental work plan for Type B materials.
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55

380
56
9.3 Type C: Thermosetting polymers
381
Thermosetting polymers include resins, epoxy, polyester, vinylesters.

Thermosetting elastomers are excluded, on the grounds that they are covered
by Material Type E.
382
It should be noted that adequate consideration should be given to the

exothermic reaction of thermosetting polymers when planning specimen
preparation. Excessive temperature rises could lead to cracking due to thermal
expansion or gas generation. Where large volumes are prepared, greater
caution is required since the sample may combust or even explode. Sample
design should attempt to avoid the trapping of heat within the sample centre - a
cooled casing may be necessary.
383
Under normal conditions, thermosetting polymers do not present a

decompression hazard during ageing testing. However, where the material is a
composite material or voids are present, appropriate measures should be
taken.
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384
PROPERTY
REQUIRE
-MENT
AGEING
REQUIRED
?
TEST
ACCEPTANCE CRITERIA
Before Ageing
After Ageing
PERMEATION TESTING
Water permeability
See Section 8.2.2
Yes
See Section 7.
Calculated release
rate (Appendix 7)
<0.25 m3/year
<50% increase
Dry mass
Measurement of
mass after drying
to constant mass at
105 oC (221 oF)
Yes
Absorption
During hardening
See Section 8.4.1
N/A
<2% by volume
Hardened
See Section 8.4.1
Yes
<5% by volume
During hardening
See Section 8.4.2
N/A
<2% by volume
Hardened
See Section 8.4.2
Yes
<2% by volume
ASTM E228
No
<1% linear strain

difference
Creep
ISO 899-1
No
<1% linear strain
Triaxial Testing
Cohesion
Poissons ratio
UCS
ISO 10426-2
Yes
>1.4 MPa (200 psi)
Tensile strength
ISO 527-1
Yes
>1 MPa (145 psi)
>1 MPa (145 psi)
Elastic modulus
ISO 527-1
Yes
Hardness
See Section 8.4.2
Yes
Shear bond strength
See Section 8.6.

Substrate rugosity
should be
measured using
ASTM D7172.
Yes
>1 MPa (145 psi)*
>1 MPa (145 psi)*
Tensile bond
strength
Fatigue life
TGA / DTA / DSC

measurement
No
No decomposition
below operating
temp.
Density
ISO 1183-1
Yes
Stress relaxation

<3% loss
Shrinkage
MECHANICAL TESTING
>1.4 MPa
(200 psi)
Bond Strength
Table 6. Experimental work plan for Type C materials.

Issue 1, July 2012
57

385
58
9.4 Type D: Thermoplastic polymers
386
Thermoplastic polymers include polyethylene, polypropylene, polyamide, PTFE,

PEEK, PPS, PVDF and polycarbonate. Thermoplastics melt above a certain
temperature. Use as a barrier material above the melting temperature is not
excluded. However, in such cases, the material must be qualified using tests
conducted at this temperature. Geopolymers are excluded, as they are a
significantly different type of material and best classified as Type A.
387
Parallel molecule alignment associated with placement may result in anisotropic

properties. Test specimens are preferably taken from a simulated placed
barrier.
388
As for thermosetting polymers, thermoplastic polymers only present a

decompression hazard during ageing testing where composite inclusions or
voids are present.
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389
PROPERTY
REQUIRE
-MENT
AGEING
REQUIRED
?
TEST
ACCEPTANCE CRITERIA
Before Ageing
After Ageing
PERMEATION TESTING
Water permeability
See Section 8.2.2
Yes
See Section 7.
Calculated release rate
(Appendix 7) <0.25
m3/year
<50% increase
Dry mass
Measurement of mass
mass at 105 oC (221
o
F)
Yes
<3% loss
Absorption
During
See Section 8.4.1
No
<2% by volume
Hardened
See Section 8.4.1
Yes
<7% by volume
During
See Section 8.4.2;

thermal shock may also
need investigation
No
Not acceptable unless

planned
Hardened
See Section 8.4.2
Yes
<0.4% by volume
expansion
ASTM E228
No
<5% linear strain

difference
Creep
ISO 899-1
No
<5% linear strain
hardening
Shrinkage
hardening
MECHANICAL TESTING
Triaxial Testing
Cohesion
Poissons ratio
yield
UCS
ISO 604
Yes
>1.4 MPa (200 psi)
>1.4 MPa (200 psi)
Tensile strength
ISO 527-1
Yes
>1 MPa (145 psi)
>1 MPa (145 psi)
Elastic modulus
ISO 527-1
Yes
Hardness
ISO 868
Yes
Shear bond
See Section 8.6.

Substrate rugosity
should be measured
using ASTM D7172.
Yes
>1 MPa (145 psi)*
>1 MPa (145 psi)*
Tensile bond
strength
Fatigue life
TGA / DTA / DSC

measurement
No
No decomposition
below operating temp.
Density
ISO 1183-1
Yes
Stress relaxation
Bond Strength
strength
Table 7. Experimental work plan for Type D materials.

Issue 1, July 2012
59

390
60
9.5 Type E: Elastomeric polymers
391
Elastomeric polymers include natural rubber, neoprene, nitrile, EPDM, FKM,

FFKM, silicone rubber, polyurethane, PUE and swelling rubbers.
392
Elastomers typically are combinations of different polymers. As a result, a

reaction between constituents may occur at certain temperatures.
393
When using a multi-component system, test specimens should preferably be

obtained from a simulated placed barrier, since simulation is likely to identify
issues relating to interaction between different components. Problems with
placement may also cause the formation of voids in multi-component systems.
394
Decompression damage to specimen during testing is possible only when

inclusions or voids are present.
395
Table 8. [overleaf] Experimental workplan for Type E materials
Issue 1, July 2012

PROPERTY
396
REQUIRE- TEST
MENT
AGEING
REQUIRED
?
ACCEPTANCE CRITERIA
Before Ageing
After Ageing
PERMEATION TESTING
Water permeability
See Section 8.2.2
Yes
See Section 7. Calculated

release rate (Appendix 7)
<0.25 m3/year
<50% increase
Dry mass
Measurement of
mass after drying
to constant mass at
105oC (221 oF)
Yes
<3% loss
Absorption
During hardening
See Section 8.4.1
No
<7% by volume
Hardened
See Section 8.4.1
Yes
<7% by volume
During hardening
See Section 8.4.2
No
Not acceptable unless

planned
Hardened
See Section 8.4.2
Yes
<2% by volume
Shrinkage
ASTM E228
No
<1% linear strain difference
Creep
ISO 899-1 / ASTM

D395
No
<50% linear strain
Triaxial Testing
Cohesion
Poissons ratio
ISRM Suggested
Method
No
UCS
BS EN ISO 604
Yes
>1.4 MPa (200 psi)
>1.4 MPa (200 psi)
Tensile strength
BS EN ISO 527-1
Yes
>1 MPa (145 psi)
>1 MPa (145 psi)
Elastic modulus
BS EN ISO 527-1
Yes
Hardness
ISO 868
Yes
Shear bond
strength
See Section 8.6.

Substrate rugosity
should be
measured using
ASTM D7172.
Yes
>1 MPa (145 psi)*
>1 MPa (145 psi)*
Tensile bond
strength
Fatigue life
TGA / DTA / DSC

measurement
No
Absence of decomposition
characteristics below
operating temperature
Density
ISO 1183-1
Yes
Stress relaxation
ASTM D395 and

NORSOK M710
Yes
<50% reduction in sealing

stress (see Section 8.4.4)
<50% reduction in
sealing stress (see
Section 8.4.4)
MECHANICAL TESTING
Bond Strength
The limit for creep of elastomeric polymers is higher than that for other materials. This is because these materials can
tolerate high magnitudes of creep without detrimental effects. *Minimum shear bond strength limit has been arrived at
based on a calculation detailed in Appendix 10.
Issue 1, July 2012
61

397
62
9.6 Type F: Formation
398
The consideration of rock formations as barrier material applies where it is

planned for movement of the formation over time to form a seal additional to, or
as a replacement for, existing barriers. Where drill cuttings are placed in a well,
this material should be qualified as Type B (non-setting grout).
399
Type F materials include any low permeability formations which are sufficiently
mobile to allow rapid closure of cracks such as claystone, shale and salt.
400
Permeable and non-mobile formations such as siltstone, sand, limestone,

basalt, granite are excluded.
Issue 1, July 2012

401
PROPERTY
REQUIRE
-MENT
AGEING
REQUIRED?
TEST
ACCEPTANCE
CRITERIA
Before
Ageing
After
Ageing
PERMEATION TESTING
Water permeability
See Section 8.2.1
Yes
See Section
7. Calculated
release rate
(Appendix 6)
<0.25 m3/year
<50%
increase
Dry mass
Measurement of mass after

drying to constant mass at 105
o
C (221 oF)
Yes
<3% loss
Absorption
During hardening
Hardened
ISRM Suggested Method
During hardening
Hardened
Shrinkage
ASTM E228
No
Creep
ASTM C512 - 10
Creep rate
determined by
application
Yes
Yes
MECHANICAL TESTING
Triaxial Testing
Cohesion
2
Poissons ratio
Yes
Yes
Yes
UCS
Yes
Tensile strength
ASTM C496
Yes
Elastic modulus
ASTM C469
Yes
Hardness
Shear bond strength
Tensile bond
strength
Fatigue life
Density
Stress relaxation
Bond Strength
Table 9. Experimental work plan for Type F materials.
Issue 1, July 2012
63

402
64
9.7 Type G: Gels
403
Type G materials include polymer gels (including cross-linked gels and

polyelectrolyte gels), polysaccharides, starches, silicate-based gels, clay-based
gels and gels consisting of diesel / clay mixtures (gunk).
404
Polyelectrolyte gels are sensitive to salts or metal ions, and so mimicking

downhole conditions in this regard during ageing testing is of great importance.
Issue 1, July 2012

405
PROPERTY
REQUIRE
-MENT
TEST
AGEING
REQUIRED
?
ACCEPTANCE CRITERIA
Before Ageing
After Ageing
PERMEATION TESTING
Water permeability
1*
See Section 8.2.1
Yes

<0.25 m3/year
<50% increase
1*
See Section 8.2.2
Yes

<0.25 m3/year
<50% increase
Dry mass
Measurement of mass
mass at 105 oC (221 oF)
Yes
<3% loss
Absorption
Absorption index
Yes
During setting
Set
During setting
See Section 8.4.2
No
<2% by volume
Set
See Section 8.4.2
Yes
0% by volume
ASTM E228
No
<1% linear strain

difference
Triaxial Testing
Cohesion
Poissons ratio
yield
UCS
Tensile strength
Elastic modulus
Hardness
Shear bond
strength
See Section 8.6.

Substrate rugosity should
be measured using
ASTM D7172.
Yes
>1 MPa (145 psi)
>1 MPa (145

psi)
Tensile bond
strength
Fatigue life
TGA / DTA / DSC

measurement
No
Absence of
decomposition
characteristics below
operating temperature
Density
Stress relaxation
Shrinkage
expansion
Creep
MECHANICAL TESTING
Bond Strength
* Evaluation must be conducted to establish whether mass transport is predominantly through flow or diffusion, and the
appropriate test methodology selected. Minimum shear bond strength limit has been arrived at based on a calculation
detailed in Appendix 10.
Table 10. Experimental work plan for Type G materials.

Issue 1, July 2012
65

406
66
9.8 Type H: Glass
407
Type H materials include solid impermeable silicate glass either in particle or

block form. Waterglass or other glass compositions that are designed to be
soluble and porous / permeable glass, such as foam glass, are excluded.
408
If glass has not been sufficiently annealed (heat treatment to remove internal
stress), then it may be susceptible to failure at low loads.
409
Thermal shock can cause glass failure by inducing thermal stress due to rapid
cooling. This results from the external surface rapidly cooling whilst the bulk of
the glass remains at an elevated temperature, due to the thermal insulation
properties of glass.
410
Silicate glass is susceptible to alkaline solutions with a pH of >12.
Issue 1, July 2012

411
PROPERTY
REQUIRE
-MENT
AGEING
REQUIRED?
TEST
ACCEPTANCE CRITERIA
Before Ageing
After Ageing
PERMEATION TESTING
Water permeability
3*
3*
Dry mass

drying to constant mass at
105 oC (221 oF)
Yes
<3% loss
Absorption
During
See Section 8.4.1
No
<2% by volume
Hardened
See Section 8.4.1
Yes
<2% by
volume
During
See Section 8.4.2;
No
<2% by volume
Hardened
See Section 8.4.2
Yes
<2% by volume
expansion
ASTM E228; thermal shock

may also need investigation
No
<1% linear
strain difference
Creep
Triaxial Testing
Cohesion
Poissons ratio
Hydrostatic
compressive yield
UCS
ISO 10426-2
Yes
>1.4 MPa (200 psi)
>1.4 MPa
hardening
Shrinkage
hardening
MECHANICAL TESTING
(200 psi)
Tensile strength
Elastic modulus
ASTM C469
Yes
Hardness
ASTM E384
Yes
Shear bond
See Section 9.6
Yes
>1 MPa (145 psi)
>1 MPa (145

psi)
Tensile bond
strength
Fatigue life
Decomposition
temperature
Density
ASTM C138
Yes
Stress relaxation
Bond Strength
strength
*Mass transport through glass is theoretically not possible, although confirmation of impermeability should be conducted as
part of the function test. Minimum shear bond strength limit has been arrived at based on a calculation detailed in
Appendix 10.
Table 11. Experimental workplan for Type H materials.

Issue 1, July 2012
67

412
413
68
9.9 Type I: Metals

Type I materials Include any pure metal or alloy, such as steel and eutectic
metals (e.g. bismuth alloys). Failure modes of metals used in barrier
applications could include corrosion, stress corrosion cracking, debonding,
creep and fatigue.
Issue 1, July 2012

414
PROPERTY
ACCEPTANCE CRITERIA
AGEING
REQUIRED
After
Before Ageing
?
Ageing
REQUIRE
TEST
-MENT
PERMEATION TESTING
Water permeability
3*
3*
Dry mass

drying to constant mass at
105 oC (221 oF)
Yes
<3% loss
Absorption
During hardening
See Section 8.4.1
<2% by volume
Hardened
See Section 8.4.1
During hardening
See Section 8.4.2; thermal

shock may also need
investigation
<2% by volume
Shrinkage
Hardened
See Section 8.4.2
ASTM E228
No
<1% linear strain

difference
Creep
ISO 204
No
<1% linear strain
Triaxial Testing
Yes
Cohesion
Poissons ratio

(triaxial) or ASTM E1876
UCS
ASTM E9
Yes
>1.4 MPa (200 psi)
>1.4 MPa
(200 psi)
Tensile strength
ISO 6892-1
Yes
<50%
reduction
Elastic modulus
ISO 3312 or ASTM E9
Yes
Hardness
ASTM E18, ASTM E10 or

ASTM E384
Yes
Shear bond strength
See Section 8.6. Substrate

rugosity should be
measured using ASTM
D7172.
Yes
>1 MPa (145 psi)
>1 MPa
(145 psi)
Tensile bond
strength
Fatigue life
TGA / DTA / DSC

measurement
No
Non-melting at
operational
temperatures
Density
ISO 3369
Yes
Stress relaxation
MECHANICAL TESTING
Bond Strength
*Mass transport through metals, other than by hydrogen is theoretically not possible, although confirmation of
impermeability should be conducted as part of the function test. Minimum shear bond strength limit has been arrived at
based on a calculation detailed in Appendix 10.
Table 12. Experimental work plan for Type I materials.
Issue 1, July 2012
69

415
70
10 References
416
1. Health and Safety Executive, A guide to the well aspects of the Offshore
Installations and Wells (Design and Construction, etc) Regulations 2006,
Second Edition, HSE Books, Sudbury, 2008
417
2. Guidelines for the suspension and abandonment of wells, Issue 4, July 2012,
Oil & Gas UK
418
3. Det Norske Veritas, Qualification Procedure for new Technology,

Recommended Practice DNV-RP-A203, Det Norske Veritas, 2001
419
4. Environmental Protection Agency, 40 CFR Parts 144 and 146: Federal

Requirements Under the Underground Injection Control (UIC) Program for
Carbon Dioxide (CO2) Geologic Sequestration (GS) Wells; Proposed Rule,
Federal Register, Vol.73, No.144, 2008, pp43492-43541
420
5. Gasda, S., Bachu, S., and Celia, M., Spatial characterization of the location
of potentially leaky wells penetrating a deep saline aquifer in a mature
sedimentary basin, in press, Environmental Geology, Vol.46, 2004, pp707-720
421
6. Horsrud, P., Estimating mechanical properties of shale from empirical

correlations, Paper (SPE 56017), SPE Drilling & Completion, June 2001
422
7. Kristiansen, T. G., Geomechanical characterization of the overburden above

the compacting chalk reservoir at valhall, Paper (SPE/ISRM 47348), Proc.,
Eurock 98, Trondheim, Norway, 1998
423
8. Fokker, P., The behaviour of salt and salt caverns, Ph.D. thesis University of
Delft, 1995
424
9. Peach, C.J., Influence of deformation on the fluid transport properties of salt

rocks, Ph. D. thesis University of Utrecht, 1991
425
10. Arnold, S.R. and Littlejohn, I., Technical Note 12 - Investigation into the
relationship between aggregate absorption and the permeability of concrete,
Royal Military College of Science, Shrivenham, 1983, 1pp
426
11. The Concrete Society, Permeability of Site Concrete A review of methods

and experience, The Concrete Society, Camberley, UK, 2008, 80pp
427
12. Lawrence, C.D., Water permeability of concrete, Concrete Society Materials

Research Seminar, Serviceability of Concrete, Slough, UK, 1985
428
13. Marion, H. and Mahfouz, C., Design and construction of the Ekofisk artificial
island, Proceedings of the Institution of Civil Engineers, Vol. 56, 1974, pp497511
429
14. Watson, A.J. and Oyeka, C.C., Oil permeability of hardened cement pastes
and concretes, Magazine of Concrete Research, Vol. 33, 1981, pp85-95
430
15. Bourbie, T. and Walls, J., Pulse decay permeability: analytical solution and
experimental test, SPE Journal, Vol.22, 1982, pp719-721
Issue 1, July 2012

431
16. Dhir, R.K., Hewlett, P.C. and Chan, Y.N., Near surface characteristics of
concrete: intrinsic permeability, Magazine of Concrete Research, Vol.41, 1989,
pp. 87-97
432
17. Paikaray, S., Banerjee, S. and Mukherjee, S., Geochemistry of shales from
the Paleoproterozoic to Neoproterozoic Vindhyan Supergroup: Implications on
provenance, tectonics and paleoweathering, Journal of Asian Earth Sciences,
Vol.32, 2008, pp34-48
433
18. US Department of Energy, Handbook of Methods for the Analysis of the

Various Parameters of the Carbon Dioxide System in Sea Water, Version 2, A.
G. Dickson & C. Goyet (eds.), US Department of Energy, Oak Ridge,
Tennessee, 1994
434
19. Dresel, P.E. and Rose, A.W., Chemistry and origin of oil and gas well brines
in Western Pennsylvania, Pennsylvania Geological Survey, 4th Series, OpenFile Report OFOG 1001.0, 2010
435
20. Leirvik, F. and Resby, J.L.M., Weathering Properties of the Alvheim Oil,
Kneler, SINTEF, Trondheim, Norway, 2007
436
21. Union Gas Website (accessed February 2011)

http://www.uniongas.com/aboutus/aboutng/composition.asp,
437
22. CEFAS Offshore Chemical Notification Scheme (accessed 2011)

http://www.cefas.co.uk/industry-information/offshore-chemical-notificationscheme.aspx
Issue 1, July 2012
71

438
11 Appendix 1: Chemical environment
439
11.1 Seawater and brine composition
440
The composition of water encountered in the well environment can vary

significantly, although the key features a high chloride, sulfate, sodium and
magnesium concentration are common. The standard mean composition of
seawater with a salinity of 35,000 mg/L (and therefore defined as saline) is
presented in Table 13.
441
An example of the composition of formation water with a brine-type salinity is

provided in Table 14, although it should be stressed that composition can vary
significantly depending on rock type and many other factors.
442
Artificial brines rich in other constituents such as bromide salts, are also used
for activities such as completion.
443
The pH of brine can vary considerably, and this can potentially have
implications for the longevity of certain materials. pH measurements of brines
from shales in one study varied from 3.9 - 9.4 [Ref 17].
Species
444
Cl
19,352
SO42-
Br
F
2,712
67
1
+
10,784
2+
1,284
2+
412
Na
Mg
Ca
K
Concentration (mg/L)
+
2+
399
Sr
B(OH)3
20
B(OH)4-
CO2
0.4
HCO3-
108
CO32-
16
OH-
0.2
Table 13. Standard mean chemical composition of seawater with a salinity of

35 mg/L [Ref 18].
72
Issue 1, July 2012

Species
445
Cl
151,000
SO42-
140
Br
F
1,210
61,900
2+
2,920
2+
24,500
Na
Mg
Ca
K
Concentration (mg / kg)
200
2+
Sr
1,420
HCO3-
43
Table 14. Chemical composition of a formation water with a brine-type salinity

[Ref 19].
446
447
11.2 Oil composition

Table 15 shows the typical types of compound found in crude oil, with very
approximate proportions. It should be stressed that proportions vary from
source to source.
Approximate proportion
Compound type
448
(% by volume)
Asphaltenes
Resins
10
Non-Hydrocarbons
Aromatics
15
Naphthenes
35
Iso-Alkanes
15
n-Alkanes
20
Hydrocarbons
Paraffins
Table 15. Chemical constituents of crude oil [Ref 20]
449
11.3 Gas composition
450
Table 16 shows ranges of concentrations of gas compounds found in fossil

natural gas. It should be stressed that there is typically large-scale variation in
gas composition from a given locality. In addition H2S may be present.
451
Where a well is used for carbon capture and storage, the composition of the
captured gas will vary depending on the process producing the CO2. Table 17
gives typical compositions of gases for capture from a range of different types
of process.
Issue 1, July 2012
73

Component
452
Range (mole %)
Methane
87.0 - 96.0
Ethane
1.5 - 5.1
Propane
0.1 - 1.5
iso - Butane
0.01 - 0.3
normal - Butane
0.01 - 0.3
iso - Pentane
trace - 0.14
normal - Pentane
trace - 0.04
Hexanes plus
trace - 0.06
Nitrogen
0.7 - 5.6
Carbon dioxide
0.1 - 1.0
Hydrogen
trace - 0.02
Table 16. Ranges of concentrations of compounds encountered in fossil natural

gas [Ref 22].
Process
453
Component
Post-combustion
with amines
Oxy-combustion
Pre-combustion coal gasification
Pre-combustion
refinery
CO2
>99 % vol
85 % vol
>95 % vol
16 % vol
O2
<150 ppmv
2 % vol
<100 ppmv
N2
<350 ppmv
0.1 % vol
<4 % vol
0.3 % vol
Ar
0.2 % vol
0.5 % vol
CO
100 ppmv
<0.1 % vol
4 % vol
NOx
<400 ppmv
SO2
<100 ppmv
CH4
<5 % vol
3 % vol
H2S
<10 ppmv
Glycol
<1500 ppmv
H2
76 % vol
H2O
0.3 % vol
Table 17. Typical compositions of gases for carbon capture and storage-based
on source process.
454
455
74
11.4 Non-native chemicals

Non-native chemicals are substances used for various purposes during well
production. These can include EOR chemicals, scale inhibitors and corrosion
inhibitors. For the UK, information relating to products used during offshore oil
and gas production can be obtained from the CEFAS Offshore Chemical
Notification Scheme [Ref 21]. Details of specific chemical constituents can be
obtained from the supplier.
Issue 1, July 2012

456
12 Appendix 2: Radiation
457
12.1 NORM activity estimates
458
The following activity levels for a range of isotopes occurring as NORM scale
are assumed under normal circumstances:
Ra-226: 40 Bq/g
Pb-210: 150 Bq/g
Ra-228: 2.5 Bq/g
Th-228: 1 Bq/g
459
If an average NORM scale thickness of 1 mm is assumed, a 5 tubing joint of

12.2 m (40 ft) would contain 7.3 kg (16 lb) of scale. Using the above activity
values the activity deriving from individual isotopes would be:
Ra-226: 320 kBq
Pb-210: 1,200 kBq
Ra-228: 20 kBq
Th-228: 8 kBq.
460
461
12.2 Lost logging tools

When a logging tool with a radioactive source is found stuck in the borehole,
extensive efforts have to be made to recover the tool. Should, in a rare event,
these efforts be unsuccessful, then the tool needs to be covered by cement and
the hole partially abandoned; a sidetrack is then drilled. The radioactivity levels
of logging tools varies. A typical value of a radionuclide is:
Caesium 137 : 2.3 TBq
Americium 241: 5 TBq.
Issue 1, July 2012
75

462
13 Appendix 3: Estimating operational pressures
463
In order to estimate the operational conditions of the permanent barrier material

over its expected life, the following procedure is suggested.
464
The force or stress acting on the top surface of the barrier can be found by
integrating the bulk density of fluids and materials above the upper surface of
the barrier. This is the same procedure as calculating overburden stress, but
within the wellbore.
465
It is assumed that, with time, the pore pressure in the barrier will equalise with
the pressure the barrier is exposed to from above and below.
466
The weight of material above the barrier will result in it expanding against the
steel pipe or the formation determined by the Poissons ratio (v) of the barrier
material. It is suggested that the average Poissons ratio determined from
triaxial testing is used for this calculation. A schematic of the situation is shown
in Figure 11.
467
Sa
Sc
Figure 11. Schematic of operational conditions of the permanent barrier.
76
Issue 1, July 2012

468
The stresses in the barrier can therefore be estimated from:
Where:
469
Sa
the stress acting on the upper surface of the barrier (Pa);
Sc
the compressive stress resulting from the barrier expanding against

the casing (Pa);
the bulk density (g/m3);
depth (m);
acceleration due to gravity (m/s2);
Poissons ratio of the barrier material;
pore pressure in the barrier (Pa); and
the depth of the upper surface of the barrier (m).
The anticipated life-of-well stresses should be used in the estimation process.

The barrier material selected should be of sufficient strength to withstand the
stresses estimated using the above estimation method.
Issue 1, July 2012
77

470
471
14 Appendix 4: Calculation of flow rates through a

microannulus.
The rate of flow (Q, units m3/s) of a fluid through a microannulus between a
barrier and casing is given by the equation:
Where:
78
is the permeability of the microannulus (m2);
wa
is the width of the microannulus (m);
xa
is the length of the barrier circumference which has separated from the
casing to form a microannulus (m);
p1-p2
is the pressure difference between the top and bottom of the barrier (Pa);
is the dynamic viscosity of the fluid (Pa.s); and
is the length of the barrier (m).
472
The example calculation considers a 30.5 m (100 ft) barrier in a 9-5/8 casing
with a pressure difference of 6.9 MPa (1,000 psi). It is assumed that the casing
has an interior diameter of 22.90 cm (9 inches) and therefore an interior
circumference of 71.9 cm. It is assumed that the microannulus extends around
the full circumference of the barrier, and has a width of 25 m and a
permeability of 5.14x10-11 m2 (52.1 darcy). It is also assumed that the fluid
below the barrier comprises only methane, with a dynamic viscosity of 1.0910-5
Pa.s. The calculation assumes the fluid is incompressible, which is not the case
in reality.
473
The influence of the microannulus width (w) on permeability can be calculated

using the equation:
Issue 1, July 2012

474
475
476
15 Appendix 5: Caprock properties

The main characteristic of cap rocks is their low permeability. The permeability
of a caprock capable of trapping hydrocarbons over geological timescales is
typically in the 1 to 0.01 microdarcy range. Caprock types with such low
permeabilities typically include shales, salt, anhydrites, well-cemented
carbonates and basement rocks (granite). The nuclear industry typically targets
soft shales, salt and unfractured granite for long term nuclear waste storage.
Cracks in the rocks can alter the sealing capability of the intact matrix and, in
general, cracks will tend to close faster in soft and weak rocks than in hard and
strong rocks.
15.1 Typical North Sea shale properties
477
A review of shales from North Sea field cores and relevant outcrop shales
shows a range of depths between 1,370 and 4,870 m (4,500 and 16,000 ft),
with porosities ranging between 55% and 3% [Ref 6]. In general, the deeper the
shale, the more compacted it is and the lower the porosity.
478
Sonic travel time or compressional wave velocity measurements made

perpendicular to the bedding plane can be used as a means of estimating
in situ shale properties including porosity, unconfined compressive strength
(UCS) and modulus of elasticity. A high velocity equates to high strength and
modulus. In the North Sea UCS varies between 3.5 and 86 MPa (500 to 12,500
psi). Modulus of elasticity varies between 0.4 and 14 GPa (60,000 psi and
2,000,000 psi).
479
A study of shales over a field in the North Sea reports permeability values
between 6.6 to 0.021 microdarcy. The permeability along the bedding of the
shale is typically at least one order of magnitude larger than the permeability
perpendicular to the bedding [Ref 7].
480
15.2 Typical North Sea salt formation properties
481
Different salt layers in the North Sea behave differently mechanically. This is
related to the composition and structure of the salt. Formations can contain
layers of various salts including halite (NaCl), carnallite (KMgCl36H2O) and
bischofite (MgCl26H2O).
482
The UCS of halite is typically between 20 to 30 MPa (3,000 to 4,400 psi), when
exposed to gas, oil or brine. Carnallite usually has a UCS of 8.5 MPa (1,200
psi), whilst that of bischofite is lower, at around 6.5 MPa (950 psi). The
presence of brine has the effect of reducing strength, with UCS values for
carnallite and bischofite dropping to 6.5 MPa (950 psi) and 2 MPa (300 psi)
respectively in these circumstances [Ref 8].
483
The permeability of salt (NaCl) is typically in the range 10 to 0.001 microdarcy

[Ref 9].
Issue 1, July 2012
79

484
485
16 Appendix 6: Flow calculations

The rate of flow (Q, units m3/s) of a fluid through a barrier is given, using
Darcys formula, as:
Where:
486
80
the permeability (m2);
the cross sectional area of the barrier (m2);
p1-p2 =
the pressure difference between the top and bottom of the barrier(Pa);
the dynamic viscosity of the fluid (Pa.s); and
the length of the barrier (m).
The example in this document considers a 30.5 m (100 ft) barrier made of
cement in a 7 casing with a pressure difference of 6.9 MPa (1,000 psi). It is
assumed that the casing has an interior diameter of 15.75cm (6.2 inches). A
value of 20 microdarcy has been used for the permeability (which is typical of
good cement). It is assumed that the fluid below the barrier comprises only
methane, with a dynamic viscosity of 1.0910-5 Pa.s. The calculation assumes
the fluid is incompressible, which is not the case in reality.
Issue 1, July 2012

487
488
17 Appendix 7: Diffusion calculations

The example calculation relating to diffusion employs Ficks law:
Where:
489
the flux per unit area (moles/m2);
the apparent diffusion coefficient (m2);
c1-c2 =
the concentration difference between the top and bottom of the barrier
(moles/m3);
the length of the barrier (m).
For the example, it is assumed that the only fluid below the barrier is methane
at a pressure of 34.5 MPa (5,000 psi). It is assumed that the partial pressure of
methane above the barrier is negligible. The concentration of gas can be
related to the pressure, or partial pressure (Px, units Pa), of a gas using the
ideal gas law equation:
or
Where:
nx
the number of moles of gas (mol);
the volume of gas (m3);
the gas constant (J/molK); and
the temperature (K).
490
Thus,
491
For the example, flux is of less interest than the actual rate of release, and so
the equation can be modified further:
Where:
A
Issue 1, July 2012
is the cross sectional area of the barrier (m2)
81

492
Finally, the release rate in mass terms can be converted to a volumetric release
rate (vrr, units m3/s), calculated for methane once at the surface (i.e. at
atmospheric pressure, Pa) using the ideal gas law equation again:
Rearranging:
The value used for atmospheric pressure was 101,325 Pa.
82
Issue 1, July 2012

493
18 Appendix 8: Relevant industry standards
494
ASTM C138 Standard test method for density (unit weight), yield, and air
content (gravimetric) of concrete
495
ASTM C469 Standard test method for static modulus of elasticity and Poisson's
ratio of concrete in compression
496
ASTM C496 Standard test method for splitting tensile strength of cylindrical
concrete specimens
497
ASTM C512 Standard test method for creep of concrete in compression
498
ASTM C1583 Standard test method for tensile strength of concrete surfaces
and the bond strength or tensile strength of concrete repair and overlay
materials by direct tension (pull-off method)
499
ASTM D395 Standard test methods for rubber property - Compression set
500
ASTM D4541 Standard test method for pull-off strength of coatings using
portable adhesion testers
501
ASTM D4943 Standard test method for shrinkage factors of soils by the wax
method
502
ASTM D7127 Standard Test Method for Measurement of Surface Roughness of

Abrasive Blast Cleaned Metal Surfaces Using a Portable Stylus Instrument
503
ASTM E9 Standard test methods of compression testing of metallic materials at

room temperature
504
ASTM E10 Standard test method for Brinell hardness of metallic materials
505
ASTM E18 Standard test methods for Rockwell hardness of metallic materials
506
ASTM E228 Standard test method for linear thermal expansion of solid
materials with a push-rod dilatometer
507
ASTM E384 Standard test method for Knoop and Vickers hardness of materials
508
ASTM E1876 Standard test method for dynamic Young's modulus, shear
modulus, and Poisson's ratio by impulse excitation of vibration
509
EN 12390 Part 8 Testing Hardened Concrete. Part 8: Depth of penetration of

water under pressure
510
EN 13121 Part 2, GRP tanks and vessels for use above ground. Composite
materials. Chemical resistance
511
ISO 204 Metallic materials -- Uniaxial creep testing in tension -- Method of test
512
ISO 527-1 Plastics -- Determination of tensile properties - Part 1: General

principles
Issue 1, July 2012
83

84
513
ISO 527-2 Plastics -- Determination of tensile properties -- Part 2: Test

conditions for moulding and extrusion plastics
514
ISO 604 Plastics - Determination of compressive properties
515
ISO 868 Plastics and ebonite - Determination of indentation hardness by means

of a durometer (Shore hardness)
516
ISO 899-1 Plastics - Determination of creep behaviour - Part 1: Tensile creep
517
ISO 1183-1 Plastics - Methods for determining the density of non-cellular

plastics - Part 1: Immersion method, liquid pyknometer method and titration
method
518
ISO 15156 / NACE MR0175 Petroleum and natural gas industries Materials
for use in H2S-containing environments in oil and gas production
519
ISO 2577 Plastics - Thermosetting moulding materials - Determination of

shrinkage
520
ISO 2578 Plastics - determination of the time-temperature limits after prolonged

exposure to heat
521
ISO 3312 Sintered metal materials and hardmetals - Determination of Young's

modulus
522
ISO 3369 Impermeable

Determination of density
523
ISO 6892-1 Metallic materials - Tensile testing - Part 1: Method of test at room
temperature
524
ISO 6892-2 Metallic materials - Tensile testing - Part 2: Method of test at

elevated temperature
525
ISO 10426-2 Petroleum and natural gas industries -- Cements and materials for
well cementing - Part 2: Testing of well cements
526
ISO 10426-5 Petroleum and natural gas industries -- Cements and materials for
well cementing -- Part 5: Determination of shrinkage and expansion of well
cement formulations at atmospheric pressure
527
ISO 11960 Petroleum and natural gas industries -- Steel pipes for use as casing
or tubing for wells
528
ISO 14310 Petroleum and natural gas industries - Downhole equipment Packers and bridge plugs
529
NORSOK M-710
manufacturers
530
ISRM Suggested method for determining the strength of rock materials in

triaxial compression, 1978
sintered
Qualification
of
metal
materials
non-metallic
and
sealing
hardmetals
materials
and
Issue 1, July 2012

531
ISRM Suggested methods for determining the indentation hardness index of

rock materials, 1998
532
ISRM Suggested method for determining the shore hardness value for rock,
2006
533
ISRM Suggested method for determining hardness and abrasiveness of rocks Part 3 Determination of the Schmidt rebound hardness, 1978
534
ISRM Suggested method for laboratory testing of argillaceous swelling rock Part 2 - Determining maximum axial swelling stress, 1989
535
ISRM Suggested method for laboratory testing of argillaceous swelling rock Part 3 - Determining axial and radial free swelling strain, 1989
536
ISRM Suggested method for Determining Water Content, Porosity, Density,

Absorption and Related Properties and Swelling and Slake-Durability Index
Properties - Part 1 - Determining Water Content, Porosity, Density, Absorption
and Related Properties, 1977
537
ISRM Suggested method for determining the uniaxial compressive strength and
deformability of rock materials - Part 1 - Determination of the uniaxial
compressive strength of rock materials, 1979
538
ISRM Suggested method for laboratory testing of swelling rocks - Part 3 Determining axial and radial free swelling strain, 1999
Issue 1, July 2012
85

539
540
541
19 Appendix 9: Cement material reference data

For reference purposes, relevant properties of a hardened neat Class G
Portland cement with a density of 1,892 kg/m3 (15.8 lb/gal) are provided in
Table 18.
Property
Units
Value
Permeability
<10
Modulus of elasticity
GPa (psi)
from 6.5 (944,000)

to 10.14 (1,470,000)
Poisson ratio
0.18 - 0.20
Cohesion
MPa (psi)
13.9 (2,014)
10 - 15
Tensile strength
MPa (psi)
from 3.65 (530) to 4.21 (610)
C (F)
110 (230)
Table 18. Properties of a hardened Class G cement.
86
Issue 1, July 2012

542
543
20 Appendix 10: Shear bond strength

The value for minimum shear bond strength has been arrived at using an
equation to describe the shear stress () required to move a barrier, which is not
bonded to the casing, out of its original position:
Where:
544
the pressure difference across the barrier (Pa);
the cross-sectional area of the barrier (m2); and
Ac
the contact surface between the barrier and the casing (m2).
Using the case of a 9-5/8 casing with an interior diameter of 21.6 cm (8.5
inches), a barrier length of 1 m (3.3 feet), and a pressure difference of 6.9 MPa
(1,000 psi), the shear stress required is 0.37 MPa. Thus, since any greater
barrier length will reduce the shear stress, a shear bond strength of 1 MPa
should be wholly adequate.
Issue 1, July 2012
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545
546
547
548
21 Appendix 11: Background to these guidelines

These guidelines were written by a subcommittee of the Well Suspension and
Abandonment (WSA) workgroup which was formerly known as workgroup 5.
The members of this subcommittee are:
Jules Schoenmakers, Shell Upstream Europe, Workgroup Chair
Simon Hough, Chevron North Sea Ltd, UK
Tom Dyer, University of Dundee, UK, Technical Author
Frans Janssen, Shell Global Solutions, Netherlands
Carl Johnson, Schlumberger, UK
Tron Golder Kristiansen, BP, Norway
Inge Carlsen, SINTEF, Norway
Preben Randbol, SINTEF, Norway
Antoine Barraque, Storengy, France
Andre Garnier, Total, France
Jean-Benoit Laudet, Total, France
The first draft of this report has been issued for comments to a number of
companies. Their comments and input is gratefully acknowledged:
Baker BJ Services, USA
BP, Norway
BP, USA
BP, UK
Chevron, USA
Halliburton, USA
ExxonMobil, UK
Los Alamos National Labs, USA
Rawwater Engineering, UK
Sandaband, Norway
Schlumberger, France
Shell, Canada
Shell, USA
SINTEF, Norway
TNO, Netherlands
WellCem, Norway
Workgroup 5 was previously part of Decommissioning Steering Group which
was formed by DECC and industry (represented by Oil & Gas UK). Recently
this group has been restructured and it was felt that workgroup 5 should be
incorporated into another Oil & Gas UK forum, the Well Life Cycle Practices
Forum (WLCPF).
549
88
The WLCPF is also the interface of choice for HSE and DECC to engage the
UK offshore industry on well-related matters. The WLCPF has representatives
from over 45 different well-operators and well management companies, and
over 60 companies have been involved in the various workgroups and review
cycles.
Issue 1, July 2012

Guidelines - Qualification of Materials For Well Suspension and Abandonment July 2012

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Guidelines on qualification of

materials for the suspension and

Guidelines on qualification of materials for the suspension and abandonment of wells

ISBN: 1 903 003 85 4

Guidelines on qualification of materials

UK Guidelines for the suspension and abandonment of wells ..................................... 13

General considerations for qualification of new technology........................... 15

Documentation requirements ........................................................................................ 17

Functional requirements of permanent barriers .............................................. 18

Removal options and reparability concepts ................................................................ 20

Typical conditions for wells in the North Sea ................................................................ 22

Estimating operational conditions of the permanent barrier ......................................... 23

Potential functional failure modes and root causes ........................................ 24

Shift in barrier position .................................................................................................. 24

Barrier leakage through the bulk material ..................................................................... 24

Fluid flow through porous media ................................................................................ 25

Diffusive leakage ........................................................................................................ 25

Leaks around the bulk material ..................................................................................... 26

External / internal stresses ......................................................................................... 28

Shrinkage and expansion ........................................................................................... 28

Chemical degradation ................................................................................................. 29

Quality of placement ................................................................................................... 30

Thermal expansion differences .................................................................................. 31

Drilling damage ........................................................................................................... 31

Definition of material types ............................................................................................ 32

Critical material properties related to potential failure modes ....................................... 32

Approach to defining acceptance criteria for mass transport properties ...... 34

Experimental work plan ..................................................................................... 36

Literature investigation .................................................................................................. 36

Permeation testing ........................................................................................................ 36

Issue 1, July 2012

Interaction with fluid ...................................................................................................... 38

Guidelines on qualification of materials

Leaching, corrosion and chemical resistance ............................................................ 38

Dimensional stability ..................................................................................................... 39

Expansion / swelling ................................................................................................... 39

Differential thermal expansion .................................................................................... 40

Creep and stress relaxation........................................................................................ 41

Mechanical testing ........................................................................................................ 41

Elastic modulus .......................................................................................................... 42

Internal friction angle .................................................................................................. 42

Poissons ratio ............................................................................................................ 43

Hydrostatic compression testing................................................................................. 43

Unconfined compressive strength (UCS) ................................................................... 43

Tensile strength .......................................................................................................... 43

Bond strength ................................................................................................................ 44

Shear bond strength ................................................................................................... 44

Tensile bond strength ................................................................................................. 45

Fatigue life ..................................................................................................................... 45

Decomposition temperature .......................................................................................... 45

Ageing testing ............................................................................................................... 46

Function test .................................................................................................................. 49

Field trial ........................................................................................................................ 51

Material types specific experimental work plans .......................................... 52

Type A: Cements, ceramics (setting) ............................................................................ 52

Type B: Grouts (non-setting) ......................................................................................... 54

Type C: Thermosetting polymers .................................................................................. 56

Type D: Thermoplastic polymers .................................................................................. 58

Type E: Elastomeric polymers ...................................................................................... 60

Type F: Formation ......................................................................................................... 62

Type G: Gels ................................................................................................................. 64

Type H: Glass ............................................................................................................... 66

Type I: Metals ................................................................................................................ 68