IMPROVEMENTS TO MATERIALS QUALIFICATION TESTING

An Update of NORSOK M-710 Rev 2

6th MERL Oilfield Engineering with Polymers Conference 2008
Glyn MORGAN, Barry THOMSON and Rod MARTIN

Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Introduction

NORSOK M-710 was developed in the 1990s to improve materials selection

and service life assessment of polymers intended for use offshore.

The procedures and intent were partly based on the MERL Seal Life JIP
sponsored by many companies present today.

Those procedures are common and relevant to the materials and

environment being evaluated and qualified.

Two aspects of material performance are addressed:

chemical ageing (usually sour)

rapid Gas Decompression (RGD)
The methodologies have been well established and many materials have been
tested.

MERL 2008

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Background

NORSOK M-710 is often the default specification for many operators.

Therefore, many service providers, component suppliers and material
suppliers now have to conform to its requirements.

Over the last 6-10 years, all involved have gained experience and the level of
polymer knowledge has increased.

MERL 2008

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Background

Therefore, further developments to NORSOK M-710 were recognised as

beneficial, based on the following issues:

incorporate new knowledge into M-710 to provide increased confidence

in materials selection and use

procedures to reflect service environments as much as possible as well as

addressing some of the practical challenges associated with the testwork
itself

materials already qualified remain so

transition of M-710 into an ISO standard would bring wider acceptance
and industry conformity to materials specification.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising NORSOK-M710 Rev. 2

AGEING - Chemical versus Physical

Physical changes (swelling, softening) occur when a fluid is absorbed into a

polymer causing reversible changes in property level.

Chemical ageing occurs as a chemically-aggressive fluid causes chemical

bonds to break or form permanently within the polymer. Property levels
change continuously and irreversibly.

Both mechanisms can occur, causing different effects over different

timescales and probably at different rates.

Background information and a procedure on how to identify and report

these phenomena is proposed to be added to Rev 3 in an accompanying
technical note/appendix.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

STEP 1 Measure property change with time at each
temperature (T black (service), blue to red)

10

Property level

0
0

10

20

30

40

50

60

Ageing time

STEP 2 Plot ln(1/t) vs 1/T and extrapolate

to service temperature and hence life

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

AGEING - Chemically Resistant Materials

Some materials are chemically resistant and their properties do not degrade
during the exposure to enable a service life prediction to be made. In other
words, only physical ageing occurs (swelling). Eg. unfilled PFTE, PEEK.

Hence it is not possible to establish an Arrhenius plot.

The Standard needs to address this situation and appropriate words are
needed which can be proposed for addition to the Standard.

MERL 2008

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

AGEING - Material Reference Points

The current control/reference point is the unaged (dry) polymer (X).

It may be more appropriate to use the oil-soaked (but unaged) material as
the reference condition (for tensile property changes); that is, Y.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

AGEING - Property Change Criteria

The Standard currently uses a 50% tensile property change as the

acceptance criterion (what is relevance of 50% change NOT being attained?)
14

85
80

12
10

65
60

ln (rate)

Property

75
70

55
50

8
6
4
2

45
40
0

100

200

300

Exposure time (days)

400

0
0.004

0.005

0.006

0.007

0.008

0.009

0.01

1/T

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

AGEING - Fluids

The current NORSOK fluid consists of an oil, water and gas mixture. The oil
has an average solubility parameter which governs its swelling tendency.

Model oils are chosen by mixing three hydrocarbon liquids representing

paraffinic (or aliphatic), naphthenic, and aromatic components.

Higher levels of H2S are now frequently encountered which can affect ageing.
It is proposed to add oils with medium and high aromaticity (10, 25 and
40%). A higher level of H2S will also be included (10%).

Completion fluids and other special fluids will be given more prominence
in the standard.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

AGEING - Checking for Ageing, Test Piece Format, Weighing and Storage

Immersion of aged specimens in a low viscosity solvent will provide an

additional check on the influence of hostile species on material crosslink
80
density. Dry first.

For elastomers, use flat sheet rather than

O-rings for ageing tests.

% Mass change

60

40

20

Develop a consistent method for removal,

weighing and storage of samples prior to
mechanical testing.

0
0

4
1/2

Time in solvent (hrs )

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

AGEING - Summary

Guidance on ageing/non-ageing situations

Service life prediction
Chemically resistant materials
Arrhenius deviations
Material reference points
Failure criterion (or criteria) for tensile properties
Oil composition
H2S level
Post-exposure determination of ageing (swelling)
Test piece format, replication level, weighing/storing procedure
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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD - Introduction

Soak Test

Leak Test

The soak test is a materials tests based on inspection which does not
necessarily signify that leakage will occur in 4/5-rated seals and not in those
rated 3 (although more likely).

NORSOK M-710 not a functional test leave that to ISO 10423 etc.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD Introduction

Relationship between RGD resistance, temperature and pressure.

Risk of RGD damage

PRESSURE
Increasing pressure

gas conc.

High
.
.
.
Medium
.
.
.
.
Low

Low

high

med

low
TE MPE RATURE
Medium
.

High

Low modulus, tear strength

outweigh high D and low gas
conc.
High modulus, tear
s trengt h outweigh
low D and high gas
conc.
D

mo d, tear str
gas solubility
Increasing tem perature

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD Introduction

Ratings for 21 compounds after 1 cycle.

5555, 5555
5555, 5444
5555, 4444
5555, 4443
5444, 4444
5430, 4110
5432, 0000
4444, 4444
4444, 4444
4410, 4400
4211, 3311
4000, 1000
4000, 1000
1000, 1000
0000, 0000
0000, 0000
0000, 0000
0000, 0000
0000, 0000
0000, 0000
0000, 0000

POOR

GOOD

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD Test Piece - O-Ring Section

Currently, the Standard test specimen shall be an O-ring seal of size No.
325 rarely used. The seal section is critical. There is little point testing
5.33 mm O-rings, if the service CS is 6.99 mm. The service section(s) should
be tested.

It cannot be assumed that if 5.33 mm passes then all sizes up to this are
qualified to the same conditions. It should be possible to justify this if the
housing details are identical. If 6.99 mm CS O-rings are being RGD-tested,
the test seals are likely to be specially moulded, since the smallest Standard
size is BS425.

A table, or series of guidelines is needed to show users the number of

variables including size which can contribute to RGD resistance and their
relationship with one another. Background info.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD Test Piece - Housing

The exposure of constrained materials is useful for obtaining information on

the materials behaviour to compare with other materials. However, it may
not be representative of how the materials will actually be used in service.

It is proposed that additional tests are added to the Standard where the
seal section and the housing geometry should represent service or, if
these are not known, representative geometries should be employed in
testing.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD Test Piece - Large O-Rings

Because of the different volume of material under test, there is a different

probability of damage zones within that volume.

In reality, larger O-rings are likely to be used in leak tests. For instance,
recent MERL leak testing used O-rings having ODs in the 40-50 mm range.
Moreover, the larger the seal, the larger the cell required to house them.

It is proposed to add the requirement for more sectioning for larger Orings, where the number of sections is related to the size (volume) of the
O-ring.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD Test Variables Gas

Currently, M-710 restricts choice of gas to three: 100% CO2, 97/3 CH4/CO2,
90/10 CH4/CO2.

From these three, a Standard mixture should be specified: 90/10 (the

most commonly used in MERL tests).

It is proposed that the gas mixture certification (if purchased) should be

part of test report.

Rev 2 also notes that sweet RGD testing qualifies for sour service as well.
This is acceptable if substitute gas equivalent to H2S. It is proposed to
explore this.

Rev 2 also assumes dry gas use, but even in gas lines there will be treatment
chemicals applied. Gas mains (low pressure) is the only obvious dry
application. It is proposed to include the use of wet gas if appropriate.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD Test Variables Temperature and Pressure

Test temp
Test pressure
Rating
max
Rating
max
A
50
1
2175
B
82
2
3000
C
100
3
4000
D
121
4
5000
E
150
5
7500
F
177
6
10000
G
200
7
15000
H
any
8
any
Current NORSOK minimum
ISO 10423 levels

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD Test Variables Soak Period

The first soak period should be long enough to saturate seals, the larger the
seal section, the longer the time that is required to soak. It is proposed
that the initial soak period is reduced for small section seals, with
justification.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD Test Variables Decompression Rate

The depressurization is usually to atmospheric pressure between cycles

(worst case but may not represent service). It is proposed that the standard
states that de-pressurisations will be to atmospheric pressure, unless
required by service conditions.
250

200

200

150
100
100

Pressure (bar)

Temperature

150

50
50

0
0

50

100

150

200

250

300

Time (hrs)
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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD - Characterisation of Damage Sectioning of O-Rings

No guidance is given where to section the seal to conduct the inspection. It

is possible to section a seal with RGD damage to avoid the damage. It is
proposed to add a requirement to section through visible damage.

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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

RGD - Characterisation of RGD Damage Damage Rating System

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Material

Improvements to Materials Qualification Testing

An Update
ABC1 Rev 2
Compound
grade of NORSOK M-710
Elastomer type
Seal manuf acturer
Lot/batch no.
Seal type
Seal size
Nominal CS
Nominal OD
Actual CS (optional)
Actual OD (optional)
RGD test conditions; requi red
Temperature
Pressure
No. of cycles
Decompression rate (mean)
Gas type
Dwell time
Housing details
Seal compression
Squeeze
Groove fill
Groove width (optional)
Groove height (optional)
Clearance (optional)
Seal replication
General
Test lab
Test date
Test gas certification Y/N
Transducer cal inf o available Y/N
P/T log available Y/N
Mean dwell time
Mean decompression rat e
Results
Crack length reference CS
NORSOK ratings

Revising of NORSOK-M710 Rev. 2

RGD - Test Certificate

REPLICATE
1
2
3
4
STAMP/SIGNATURE

HNBR
Acme Seals, Inc
2344rw4r/07
O-ring
BS 324
mm
mm
mm
mm

5.33
44.95
5.35
44.89
120
350
10
20
90/10 CH4/CO2
1

C
bar
bar/min
hr

radial
13
70

radial/axial
%
%
mm
mm
mm

hour
bar/min

Ace Test Company

10-15 August 2008
YES
YES
YES
1.05
19
actual

nominal/actual

RATING
3000, 2000, 1000, 0000
1110, 1000, 1000, 1000
1100, 1100, 1100, 0000
3120, 1000, 0000, 0000

MERL 2008

PASS/ FAIL
PASS
PASS
PASS
PASS
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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Revising of NORSOK-M710 Rev. 2

Test Plan

To validate all these points, a large test plan has been embarked upon, the
details of which are in the paper. In summary:
AGEING

RGD

Aromaticity, % H2S

Align conditions across Standards

Chemical vs physical. Mech. ref. point

Does big CS qualify smaller sections?

Failure criteria >> service life predictn

Squeeze, groove fill, housing design

Curve fitting methods

Large diameter rings (sectioning)

Ageing check

H2S substitute

Weighing/storage procedure

Decompn rate, ramped, to > atmos. P

Dwell time, no. cycles, 1 and 5 cycle
Degas conditions
Damage characterisation
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Improvements to Materials Qualification Testing An Update of NORSOK M-710 Rev 2

Summary

The intention of the JIP is to produce a comprehensive and robust revision of

NORSOK M-710 that can be understood by novice specifying engineers and
polymer experts alike.

Changes implemented will be reinforced by testwork.

This experience will be used to support ISO TC67 WG7 to draft the
documents for ISO 23936 Parts 1 (Thermoplastics) and 2 (Elastomers).

Once these ISO documents are accepted, NORSOK M-710 will be phased out.

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