CLEO ISO 13628-6 Manual Issue 2

1

Environmental Oil BasedSubsea Control Fluid (HP/HT)

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

Issue 02: 7th May 2015

Prepared by: D. Gleeson

Walter Leigh Way, Moss Industrial Estate,Leigh, Lancashire, WN7 3PT, UK

+44 (0)8452 967 751

tech@offshore‐oils.com

www.offshore‐oils.com

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1.0 – INTRODUCTION

This document summarises a cross‐section of the technical data gathered to date, both within

Offshore Environmental Oils Laboratories, and using independent third parties, on CLEO

Environmental Oil Based Subsea Fluid (HT/HP).

This manual summarises some of the key technical parameters of the fluid and includes all

relevant ISO 13628‐6 (2012) Annex C criteria along with a wide range of additional materials

tested.

This data provides a broad technical review on the Technical Performance of CLEO Environmental

Oil Based Subsea Fluid (HT/HP) and will also demonstrate our commitment to producing superior

products that offer a real technical and environmental advance for this market sector.

Offshore Environmental Oils are committed to providing outstanding technical support for our

customers and some of the testing detailed in this manual are on‐going, and will be updated

regularly.

The information in this document is confidential and must not be reproduced or disclosed without

the prior permission of Offshore Environmental Oils Limited.

DOCUMENT REVISION HISTORY

Issue No. Revision Issue Date Authorised by Position

1 0 December 2012 D. Gleeson R&D Manager

2 0 May 2015 D. Gleeson R&D Manager

Please note that this document is subject to revision on a regular basis. Please ensure you have

the latest revision before using this data in applications of a critical nature.

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2.0 – PRODUCT OVERVIEW

CLEO High Temperature Environmental Oil Key Competitive Parameters

CLEO is a High Temperature Environmental Oil based Subsea Fluid.

CLEO was developed to bridge the technology gap between water based fluids and the extreme

HT/HP developments of the future by providing a very stable high temperature fluid capable of

maintaining temperatures in excess of 250°C for a project lifetime.

In addition, with the potential future requirements for closed loop systems in some sectors this

environmental oil is not only acceptable for direct discharge to sea but is designed to offer all the

properties of traditional oil based fluids in closed loop systems.

CLEO has a comparatively low viscosity for an oil based fluid which is useful when the fluid is to be

used in fields with long step‐outs.

CLEO is fully compatible with Brayco Micronic SV/3 and SV/B and can be used to replace such

fluids in existing systems where a stronger focus on environmental discharge is required.

This manual summarises some of the key technical parameters of the fluid and includes all

relevant ISO 13628‐6 (2012) Annex C criteria along with a wide range of additional materials

tested. Further updates will be available in future as fresh data becomes available.

Information given in this publication is

based on Technical Data gained in our own

and other laboratories and is believed to be

true. However, if the material is used in

conditions beyond our control, we can

assume no liability for results obtained or

damaged incurred through the application

of the data present herein.

Certified ISO 9001‐2008 For the Development, Manufacture

and Supply of Speciality Chemicals

Certificate No: 2906

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2.1 – ISO 13628‐6 (2012) ANNEX C – SUMMARY.

C.1 General Information – testing complied with specification.

C2 Test Specifications – testing complied with specification.

C.3 Thermal Stability (High Temperature) – Complies with specification after 6 months at 250 °C.

C.4 Thermal Stability (Low Temperature) – Complies with specification after 1 month at ‐25 °C.

C.5 Thermal Stability in presence of sea water – required for water glycol fluids only.

C.6 Sea Water Compatibility – required for water glycol based fluids only.

C.7 Sea Water Compatibility Specific for Synthetic Fluids only:‐

Saturation point – Complies with specification.

Static Testing With Sea Water – Complies with specification.

Dynamic Testing with Sea Water – Complies with specification.

Dewatering Capability of fluid – Complies with specification.

Water Absorption test – % Saturation as a function of time complies with specification.

C.8 Control fluid Compatibility – Complies with Specification.

C.9 Completion Fluid Compatibility – Complies with Specification.

C.10 Compatibility with Miscellaneous Operational Fluids – Complies with Specification.

C.11 Metal Compatibility with and without 10% Sea Water – Complies with specification.

AISI 316 Compatibility with CLEO and 10% Natural Sea Water – Complies with Specification.

Metal Compatibility with CLEO at 250 °C – AISI 316 complies with specification, 17‐4‐PH is not recommended for use at 250 °C. We on not recommended the use of either material at 250 °C particularly if sea water ingress is likely. We recommend that the inclusion of these materials in the ISO 13628‐6 specification should be reconsidered in light of the new higher temperatures reached by CLEO.

C.12 Elastomer Compatibility – Complies with specification.

C.13 Thermoplastic Compatibility – testing in progress.

C.14 Filterability – Complies with specification.

C.15 Fluid Lubricity and wear – Complies with specification.

C.16 Bacterial and Fungal resistance – Required for water glycol based fluids only.

C.17 Acid Buffer Capacity – Required for water glycol based fluids only.

C.18 Metal Ion Compatibility – Required for water glycol based fluids only.

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TABLE OF CONTENTS

Page

1.0 – INTRODUCTION 2

2.0 – PRODUCT OVERVIEW 3

2.1 – ISO 13628‐6 (2012) ANNEX C – SUMMARY. 3

3.0 – TYPICAL PHYSICAL PROPERTIES 8

3.1 – Physical Properties Summary 8

3.2 – Kinematic Viscosity versus Temperature Profile 9

3.3 – Density versus Temperature Profile 9

3.4 – Dynamic Viscosity versus Pressure Profile @ 4 °C 10

3.5 – Density versus Pressure Profile @ 4 °C 10

3.6 – Bulk Modulus versus Pressure Profile @ 4 °C 11

3.7 – Instantaneous Compressibility versus Pressure Profile @ 4 °C 11

3.8 – Relative Volume versus Pressure Profile @ 4 °C 12

4.0 – PRODUCT TEST SPECIFICATIONS 13

4.1 – Thermal Stability 13

4.1.1 – Thermal Stability – Accelerated Aging 13

4.2 – Thermal Stability ‐ Low Temperature 16

4.2.1 – Thermal Stability at 5 °C and ‐25 °C for 1 month 16

4.3 – Seawater Compatibility for Synthetic Fluids 16

4.3.1 – Determination of the Saturation Point of the Synthetic Fluid 16

4.3.2 – Seawater Compatibility under Static and Dynamic Conditions 18

4.3.3 – Dynamic Testing With Sea Water 21

4.3.3.1 – Dynamic Sea Water Testing – 79% v/v CLEO : 1% v/v Sea Water 22





4.3.4 – Dewatering Capability of Synthetic Fluid 27

4.3.5 – Water Absorption Test 30

4.4 – Control Fluid Compatibility 32

4.4.1.a – CLEO Compatibility with Pelagic 100 @ 5 °C 34

4.4.1.b – CLEO Compatibility with Pelagic 100 @ 20 °C 36

4.4.1.c – CLEO Compatibility with Pelagic 100 @ 70 °C 38

4.4.2.a – CLEO Compatibility with Transaqua HT‐2 @ 5 °C 40

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4.4.2.b – CLEO Compatibility with Transaqua HT‐2 @ 20 °C 42

4.4.2.c – CLEO Compatibility with Transaqua HT‐2 @ 70 °C 44

4.4.3.a – CLEO Compatibility with Oceanic HW443 @ 5 °C 46

4.4.3.b – CLEO Compatibility with Oceanic HW443 @ 20 °C 48

4.4.3.c – CLEO Compatibility with Oceanic HW443 @ 70 °C 50

4.4.4.a – CLEO Compatibility with Transaqua HC‐10 @ 5 °C 52

4.4.4.b – CLEO Compatibility with Transaqua HC‐10 @ 20 °C 54

4.4.4.c – CLEO Compatibility with Transaqua HC‐10 @ 70 °C 56

4.4.5.a – CLEO Compatibility with Brayco Micronic SV/B @ 5 °C 58

4.4.5.b – CLEO Compatibility with Brayco Micronic SV/B @ 20 °C 60

4.4.5.c – CLEO Compatibility with Brayco Micronic SV/B @ 70 °C 62

4.4.6.a – CLEO Compatibility with Pelagic 100HC @ 5 °C 64

4.4.6.b – CLEO Compatibility with Pelagic 100HC @ 20 °C 66

4.4.6.c – CLEO Compatibility with Pelagic 100HC @ 70 °C 68

4.4.7.a – CLEO Compatibility with Brayco Micronic SV/3 @ 5 °C 70

4.4.7.b – CLEO Compatibility with Brayco Micronic SV/3 @ 20 °C 72

4.4.7.c – CLEO Compatibility with Brayco Micronic SV/3 @ 70 °C 74

4.5 – Completion Fluid Compatibility 76

4.5.1.a – CLEO Compatibility with Calcium Chloride Brine 11.2 ppg (Lab Made) @ 5 °C 78

4.5.1.b – CLEO Compatibility with Calcium Chloride Brine 11.2 ppg (Lab Made) @ 20 °C 80

4.5.2.a – CLEO Compatibility with Calcium Bromide Brine 12.5 ppg (Lab Made) @ 5 °C 82

4.5.2.b – CLEO Compatibility with Calcium Bromide Brine 12.5 ppg (Lab Made) @ 20 °C 84

4.5.3.a – CLEO Compatibility with Zinc Bromide Brine 19.2 ppg (Lab Made) @ 5 °C 86

4.5.3.b – CLEO Compatibility with Zinc Bromide Brine 19.2 ppg (Lab Made) @ 20 °C 88

4.5.4.a – CLEO Compatibility with Cabot Potassium Formate Buffered 1.57 SG @ 5 °C 90

4.5.4.b – CLEO Compatibility with Cabot Potassium Formate Buffered 1.57 SG @ 20 °C 92

4.5.5.a – CLEO Compatibility with Cabot Caesium Formate Buffered 2.20 SG @ 5 °C 94

4.5.5.b – CLEO Compatibility with Cabot Caesium Formate Buffered 2.20 SG @ 20 °C 96

4.6 – Compatibility with Miscellaneous Operational Fluids 98

4.6.1.a – CLEO mixed with 35% HCl @ 5 °C from BDH ‐ Analar grade 100

4.6.1.b – CLEO mixed with 35% HCl @ 20 °C from BDH ‐ Analar grade 102

4.6.2.a – CLEO mixed with methanol @ 5 °C from Sigma Aldrich ‐ ACS grade 104

4.6.2.b – CLEO mixed with methanol @ 20 °C from Sigma Aldrich ‐ ACS grade 106

4.6.3 – CLEO mixed with MEG from Niche Products Manufacturing Plant 108

4.6.4.a – CLEO mixed with HDEO @ 5 °C 112

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4.6.4.b – CLEO mixed with HDEO @ 20 °C 114

4.6.5 – CLEO Compatibility with Silicone Oil (99:1 Ratio) 116

4.7 – Metal Compatibility 117

4.7.1 – Metal Compatibilities at 70 °C 117

SUMMARY OF METAL RESULTS FOR CLEO AT 70 °C 119

4.7.1.1.a ‐ CLEO (Neat) ‐ Multiple Piece Corrosion Testing (3 week data) 121

4.7.1.1.b ‐ CLEO (Neat) ‐ Multiple Piece Corrosion Testing (6 week data) 122

4.7.1.1.c ‐ CLEO (Neat) ‐ Multiple Piece Corrosion Testing (12 week data) 123

4.7.1.2.a ‐ CLEO with 10% Sea Water ‐ Multiple Piece Corrosion Testing (3 week data) 124

4.7.1.2.b ‐ CLEO with 10% Sea Water ‐ Multiple Piece Corrosion Testing (6 week data) 125

4.7.1.2.c ‐ CLEO with 10% Sea Water ‐ Multiple Piece Corrosion Testing (12 week data) 126

4.7.2 – Further Metal Compatibilities at 70 °C 126

4.7.2.1.a ‐ CLEO (Neat) Metals Compatibility at 70 °C (3 week data) 127

4.7.2.1.b ‐ CLEO (Neat) Metals Compatibility at 70 °C (6 week data) 132

4.7.2.1.c ‐ CLEO (Neat) Metals Compatibility at 70 °C (12 week data) 138

4.7.2.2.a ‐ CLEO with 10% Sea Water ‐ Metals Compatibility at 70 °C (3 week data) 144

4.7.2.2.b ‐ CLEO with 10% Sea Water ‐ Metals Compatibility at 70 °C (6 week data) 149

4.7.2.2.c ‐ CLEO with 10% Sea Water ‐ Metals Compatibility at 70 °C (12 week data) 155

4.7.3 ‐ AISI 316 Compatibility with Production Control Fluid and 10% Natural Sea Water 161

4.7.4 – Metal Compatibility at 250 °C 163

4.7.4.a – CLEO (Neat) Metal Compatibility at 250 °C (2 Month Data) 164

4.7.4.b ‐ CLEO (Neat) Metal Compatibility at 250 °C (6 Month Data) 165

4.7.5 – Additional Metal compatibility at 250 °C 166

4.7.6 –CLEO with 10% Sea Water Metal Compatibility at 250 °C 170

4.8 – Elastomer Compatibility 171

4.8.1 – Elastomer Compatibility 171

SUMMARY OF ELASTOMER RESULTS 172

Elastomer Compatibility with CLEO at 70 °C 175

Elastomer Compatibility with CLEO at 250 °C 179

4.9 – Fluid Lubricity and Wear 180

4.9.1 – 4 Ball Weld Point Load 180

4.9.2 – One Hour 4 Ball Wear Test 181

4.10 – Filterability 181

4.11 – Bacterial & Fungal Resistance with Seawater 182

4.11.1 – CLEO with Contaminated Sea Water at 20 & 40 °C 183

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4.11.2 – CLEO with Uncontaminated Sea Water at 20 & 40 °C 185

3.0 – TYPICAL PHYSICAL PROPERTIES

3.1 – Physical Properties Summary

Property CLEO Test Method

Viscosity (cSt)

ASTM D445

IP71

ISO 3104

@‐20 °C 154

@ 0 °C 37.0

@20 °C 14.6

@40 °C 8.5

@60 °C 5.3

@100 °C 2.3

Pour Point <‐40 °C IP15

Specific Gravity (gcm‐3)

20 0.914 IP365

Appearance Transparent, colourless / pale

yellow liquid

Flash Point / °C >200 °C ASTM D92 / IP36

Upper Temperature Stability 250 °C

Cleanliness Level

(Minimum)

17/14/12 ISO 4406

NAS 6 NAS 1638

6B/6C/6D/6E/6F SAE AS4059

Shell 4 Ball Mean Wear Scar Diameter 0.600

mm.

IP239/01 1 hour duration, 1475rpm

rotation, 30 kgf load

Solubility in Water Insoluble

Solubility in Mineral / Crude Oil

Soluble

Coefficient of Thermal Expansion m3/m3°C

0.0008

Bulk Modulus N/m2 (x109) 1.73

Falex, Shell 4 Ball, coefficient of thermal expansion and bulk modulus testing were all conducted

by independent laboratories.

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3.2 – Kinematic Viscosity versus Temperature Profile

CLEO Kinematic Viscosity as a function of temperature

Temperature / °C Viscosity / cSt

‐30 250.4

‐20 154.0

‐10 58.9

0 35.7

10 21.4

20 14.6

30 10.5

40 8.5

50 6.4

60 5.3

70 4.1

80 3.2

90 2.6

100 2.3

125 1.8

150 1.4

3.3 – Density versus Temperature Profile

CLEO Density as a function of temperature

Temperature / °C Density /g cm‐3

‐30 0.942

‐20 0.937

‐10 0.932

0 0.926

10 0.919

20 0.914

30 0.905

40 0.898

50 0.889

60 0.881

70 0.871

80 0.865

90 0.861

100 0.858

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3.4 – Dynamic Viscosity versus Pressure Profile @ 4 °C

3.5 – Density versus Pressure Profile @ 4 °C

20

30

40

50

60

70

80

90

100

110

120

0 100 200 300 400 500 600 700

Dynam

ic Viscocity (cP)

Pressure (Bara)

0.920

0.925

0.930

0.935

0.940

0.945

0.950

0.955

0.960

0.965

0 100 200 300 400 500 600 700

Density (gcm

‐3)

Pressure / Bara

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3.6 – Bulk Modulus versus Pressure Profile @ 4 °C

3.7 – Instantaneous Compressibility versus Pressure Profile @ 4 °C

0.50

0.75

1.00

1.25

1.50

1.75

2.00

0 100 200 300 400 500 600 700

Bulk M

odulus (N m

‐2x 109)

Pressure / Bara

40

50

60

70

80

90

100

110

120

130

0 100 200 300 400 500 600 700

Instan

taneous Compressibility (x 10‐6Bar ‐1)

Pressure / Bara

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3.8 – Relative Volume versus Pressure Profile @ 4 °C

0.955

0.960

0.965

0.970

0.975

0.980

0.985

0.990

0.995

1.000

1.005

0 100 200 300 400 500 600 700

Relative Volume

Pressure / Bara

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4.0 – PRODUCT TEST SPECIFICATIONS

4.1 – Thermal Stability

4.1.1 – Thermal Stability – Accelerated Aging

This test shall be performed whenever the control system operating fluid is intended for service

above 80°C (176°F).

METHODS AND MEASUREMENTS

The neat fluid is exposed at the maximum temperature specified by the fluid supplier plus a safety

margin of 10 °C (18 °F), or at the maximum operational temperature for a specific subsea project

plus the same safety margin.

Fluid is exposed for 2, 6 and 12 months. The approval can be issued after 6 months, but the test

shall continue through to 12 months to verify the 6 months result.

Visual inspection of fluid and solids formed, viscosity, lubricity, and final fluid volume are all

measurements used to validate the thermal stability.

PROCEDURE

Select aging vessels that are of 316 or better quality stainless steel for wetted components. An

inner lining of PTFE is recommended.

Clean the three test vessels/liners in accordance with ISO 3722 and for the final rinse use either

filtered de‐ionized water for water‐based fluids or filtered petroleum spirit for oil‐based fluids. Let

the vessels dry in a clean lint‐free environment. Do not use an air line to dry the vessels, as this

introduces contamination. Test for vessel cleanliness by filling with 150 ml (9.15 in3) de‐ionized

water (petroleum spirit for oil‐based fluid test), agitate, and then count particles. The acceptance

criterion is less than 150 particles greater than 5 μm per 100 ml (6.1 in3) of fluid volume.

Fill vessels with a minimum of 400 ml (24.4 in3) of the control fluid.

Purge the air space above the control fluid with dry filtered nitrogen and regulate the pressure to

a value sufficient to prevent boiling of the control fluid. Maintain this pressure throughout the

test.

Heat the vessels to the desired temperature and maintain ± 1% throughout the test.

A minimum of three 400 ml (24.4 in3) fluid samples are exposed for 2 months, 6 months and 12

months, in a separate vessel for each period. After testing the whole content of the vessels is

retrieved. This includes the liquid as well as any solids which may have collected at the bottom or

walls and cover of the vessel. After retrieval of the sample from the autoclave, any solids are

collected, dried and weighed to the nearest mg according to ISO 4405. A volume of 200 ml (12.2

in3) from each sample is reserved for the low‐temperature stability testing, (see 4.2)

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The appropriate measurements are carried out and changes relative to the unused fluid are

calculated. To avoid changes in the fluid properties after the vessel has been opened; the visual

observations are done within 8 h after opening of the vessel, and shall be documented by photos.

Test for fluid lubricity and wear (see section 4.9) before and after exposure to the maximum

temperature.

ACCEPTANCE CRITERIA

The acceptance criteria are as follows.

Visual appearance: The fluid shall not change significantly in appearance. Fading of the

initial colour is acceptable.

Fluid separation: No secondary liquid phase and no substantial amount of particles/sludge

shall form in the fluid. Maximum content of collected solids (deposits) shall not exceed

100 mg/l of fluid.

Lubricity: Lubricity shall comply with the acceptance criteria in the fluid lubricity and wear

section 4.9.

Viscosity: The viscosity shall not change by more than 10%.

Fluid volume: The retrieved volume of the fluid shall be at least 99% of the original

volume.

RESULTS

The results after ageing CLEO for six months are tabulated below and are all within acceptable

limits.

Aging Time

Appearance (relative to unused fluid)

Qualitative description of separation in

fluid e.g. Multiple phases or solids

Weight of solids recover

ed (mg/L of fluid)

Specific Gravity @ 20°C

Lubricity (IP239 Shell 4 ball, 1 h wear test, 30 kg load,

1460 rpm) Mean Wear Scar

Diameter

Weld Load / kg

Viscosity @ 40 °C /

cSt

% of fluid recovered from pod

None Clear and bright colourless / pale yellow product

None N/A 0.916 0.600 mm 250 8.4 N/A

2 months

Clear and bright orange / amber

fluid None

36.5 mg/L

0.91 0.623 mm 250 8.53 99.0%

6 months

Clear and bright orange / amber

fluid None

37.1 mg/L

0.912 0.627 mm 200 8.28 99.5%

The full datasets for the 4 ball testing are tabulated below.

Lubricant

Aging Time

and

Temperature

/ °C

Scar

Diameter

Rubbing

Direction

Ball 1 (mm)

Scar

Diameter

Right Angle

Direction

Ball 1 (mm)

Scar

Diameter

Rubbing

Direction

Ball 2 (mm)

Scar

Diameter

Right Angle

Direction

Ball 2 (mm)

Scar

Diameter

Rubbing

Direction

Ball 3 (mm)

Scar

Diameter

Right Angle

Direction

Ball 3 (mm)

Average

Scar

Diameter

MWSD (mm)

Comments

CLEO None 0.72 0.48 0.70 0.48 0.72 0.50 0.600 Wear scars asymmetric

CLEO 250°C,

2 months 0.60 0.66 0.58 0.66 0.58 0.66 0.623

Wear scars

asymmetric

CLEO 250 °C, 6 months

0.60 0.66 0.60 0.64 0.60 0.66 0.627 Wear scars

asymmetric

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The samples aged for 2 or 6 months were then aged at 5 and ‐25 °C for weeks, and showed no

changes in appearance from the recovered fluid as shown below.

Aging time @250 °C

Initial Appearance Appearance of CLEO after aging at 250 °C followed by

No further aging Aging for 1 month, 5 °C Aging for 1 month, ‐25 °C

2 months

Colourless / pale yellow fluid.

Yellow, clear and bright fluid.

Yellow, clear and bright fluid. No significant

difference after cooling.

Yellow, clear and bright fluid. No significant


6 months

Colourless / pale yellow fluid.

Amber, clear and bright fluid.

Amber, clear and bright fluid. No significant


Amber, clear and bright fluid. No significant


CLEO has undergone extensive accelerated aging testing based on the procedures laid out in ISO

13628‐6 2012 Annex C and is considered fit for service at temperatures as high as 250 °C.

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4.2 – Thermal Stability ‐ Low Temperature

4.2.1 – Thermal Stability at 5 °C and ‐25 °C for 1 month


The neat fluid and fluid samples retrieved from the high‐temperature testing are exposed for 4

wk. The appearance of the fluid is observed.

PROCEDURE

The fluid is left undisturbed for 4 weeks at 5 °C ( 41°F) and at the minimum recommended

temperature, but not lower than ‐25 °C. At the end of exposure the fluid is inspected (by naked

eye) with respect to changes in appearance including formation of liquid or solid separation.

RESULTS

Test completed. CLEO passed at all temperatures.

Product Aging

Temperature Aging Time

Appearance (relative to unused fluid ‐ at test

temperature)

Appearance (relative to unused fluid ‐ warmed to ambient)

Pass / Fail

CLEO Initial Sample None Clear and bright, colourless /

pale yellow liquid Clear and bright, colourless /

pale yellow liquid Pass

CLEO +5 °C 1 week Clear and bright, colourless /



CLEO ‐25 °C 1 week Clear and bright, colourless /



CLEO +5 °C 1 month Clear and bright, colourless /



CLEO ‐25 °C 1 month Clear and bright, colourless /



4.3 – Seawater Compatibility for Synthetic Fluids

Four tests are required to investigate the tolerance of synthetic fluids to seawater:

Determination of the saturation point of the synthetic fluid

Investigate seawater compatibility under static and dynamic conditions

Determine the dewatering capability of the synthetic fluid

Water absorption test.

Note: Artificial seawater (ASTM D1141‐98) shall be used.

4.3.1 – Determination of the Saturation Point of the Synthetic Fluid

METHODS AND MEASUREMENTS:

A quantity of artificial seawater is added to the oil and dissolved. Absolute water content and %

saturation are measured and from this the saturation point of the oil is determined.

This test should be carried out in clear plastic bottles. If glass bottles are used, the added water

will adsorb to the vessel and may lead to false results. Water does not adsorb onto plastic.

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Note readings of % saturation are not instantaneous. It will take time for the moisture in the oil to

interact with the sensor. Whilst taking a reading, stir the oil so that fluid is flowing past the sensor,

until the % saturation reading has stabilised.

PROCEDURE

Take a sample of the oil and measure the % saturation of the oil at 20°C and determine its

absolute water content by Karl Fischer. Estimate how much seawater to add to achieve a %

saturation of 80 to 85% at 20°C.

Add the appropriate quantity of artificial seawater to the oil sample, making sure that the drops

of water head to the bottom of the bottle.

Put the bottle into a normal laboratory ultrasonic bath and then gently swirl the bottle as the

“mist” of tiny droplets rises away from the larger drops of water. Do this until the “mist” is no

longer visible. This can take 30 minutes or more. After this, put the bottle on a magnetic stirrer or

bottle roller for minimum 12 hours (e.g. overnight). This will allow the tiny droplets to dissolve

fully.

Finally measure the % saturation at 20°C. If the % saturation is above 85% add fresh oil and allow

it to mix thoroughly, sufficient to bring it to the 80 – 85% target. Re‐measure the % saturation at

20°C and the absolute moisture content (Karl Fischer).

ACCEPTANCE CRITERIA

There are no acceptance criteria for this test.

RESULTS

The Plot of % saturation as a function of absolute sea water content for CLEO and Sea Water is

shown overleaf.

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Plot of % saturation as a function of absolute sea water content for CLEO and Sea Water

4.3.2 – Seawater Compatibility under Static and Dynamic Conditions

STATIC TESTING

Carefully add, without mixing, 5% and 10% (by weight) of artificial seawater to the synthetic fluid.

Record the initial observations. The mixtures are then exposed at 5, 20 and 70°C for 4 weeks. The

appearance of the mixtures are recorded weekly and compared with the neat fluid.

Use a suitable jar with a lid for the test.

METHODS

Visual inspection.

ACCEPTANCE CRITERIA

No visual solids sedimentation.

RESULTS

Test Complete.

CLEO remained clear and bright at both 5 and 20 °C throughout the test. At 70 °C CLEO also

remains clear and bright; however it then becomes hazy on cooling do to the fluid being fully

saturated with sea water.

0

10

20

30

40

50

60

70

80

90

100

0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000

% Saturation

Absolute Water Content / ppm

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Aging of CLEO with 5 or 10% Sea Water at 5, 20 and 70 °C

Product Sea Water

Addition % w/w Aging

temperature / °C Aging Time / weeks

Appearance

CLEO 5 5 1 Two phases, both are colourless, clear and bright.
















CLEO 5 70 1 Two phases, both are colourless, clear and bright. On cooling the

upper organic phase becomes slightly hazy.















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20

Aging of CLEO with 5 or 10% Sea Water at 5, 20 and 70 °C

Aging Time

5 °C 20 °C 70 °C

5% Sea Water 10% Sea Water 5% Sea Water 10% Sea Water 5% Sea Water 10% Sea Water

1 week

2 weeks

3 weeks

4 weeks

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21

4.3.3 – Dynamic Testing With Sea Water

This test closely follows the ASTM D1401 – Water separability of Petroleum Oils and Synthetic

Fluids. Artificial seawater (ASTM D1141‐98) is mixed with the synthetic fluid using a high‐speed

paddle. The mixing is stopped and observations are made at various time intervals.

METHODS

Visual inspection over time.

PROCEDURE

Following the ASTM D1401 method, use the following mixing ratios:

1, 2, 4, 8 and 40 ml of artificial seawater, made up to a total of 80ml using the synthetic fluid.

Run the ASTM D 1401 at 5°C, for 5 minutes at required paddle speed. Stop the paddle at the

required time and make observations of the mixture separation over the times specified in the

ASTM D 1401.

ACCEPTANCE CRITERIA

No visual solids sedimentation.

RESULTS

Test Complete.

CLEO conforms to the ISO 13628‐6 2012 Annex C specification as no solids are seen upon testing.

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4.3.3.1 – Dynamic Sea Water Testing – 79% v/v CLEO : 1% v/v Sea Water

Time / Minutes ml Oil –

ml Emulsion – ml Water Appearance

2 79 – 0 – 1 Aeration of oil phase seen giving trace hazy appearance. Sea water clear and bright.










Time / Min CLEO Time / Min CLEO

2

25

5 30

10

40

15

50

20

60

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15 78.5 – 0 – 1.5 Aeration of oil phase seen giving trace hazy appearance. Sea water clear and bright.








2 25

5

30

10

40

15 50

20

60

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2 25

5

30

10

40

15

50

20 60

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2

25

5

30

10

40

15 50

20

60

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2 40 – 0 – 40 Aeration of oil phase seen giving trace hazy appearance. Sea water clear and bright. Well

defined interface. Complete separation.

5 40 – 0 – 40 Complete separation after 2 minutes








Time / Min CLEO Time / Min CLEO Time / Min CLEO

2

15 30

5

20 40

10

25 120

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4.3.4 – Dewatering Capability of Synthetic Fluid

The purpose of this section is to verify that the moisture absorption process is reversible.

Note: It is recommended that this testing is carried out by a specialist company supplying drying

equipment to the offshore industry.

METHODS

Water content (ppmw) and % saturation measurement by suitable methods, check with fluid

supplier.

PROCEDURE

This will depend on the qualification procedure of the external specialist company. In principle, a

sample of the synthetic fluid will be dosed above the saturation point with artificial seawater. The

sample will then be run through the drying equipment at 20 °C (±5 °C), and samples taken

periodically for % saturation, using the moisture sensor and water content (ppmw).

ACCEPTANCE CRITERIA

After 35 circulations of the test fluid, the moisture level shall as a minimum have fallen from 80%

to 30% of the saturation point, as determined in section 4.3.1.

RESULTS

Tests were carried out using a Pall HPN021 oil drying unit, with a fluid flow rate of 21 L min‐1 and a

typical vacuum of 0.7 Bar.

The moisture level equivalent to 80% saturation of CLEO was determined as 2500 ppm water,

with 30% saturation equivalent to 200 ppm water.

The drying test was carried out in triplicate and the results are shown overleaf.

The results show that CLEO meets the requirements in ISO 13628‐6 2012 Annex C as the water

content is reduced from >80% saturation to <30% saturation within the 35 cycle limit.

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Drying of CLEO versus Saturation (Full Dataset)

Drying of from 83% Saturation Showing Reproducibility

10

20

30

40

50

60

70

80

90

100

0 5 10 15 20 25 30 35 40

% Saturation

Number of Cycles

Drying of CLEO with Synthetic Sea Water

Run 1 ‐ Start 83% Saturation

Run 2 ‐ 92% Saturation start

Run3 ‐ 84% Saturation at start

10

20

30

40

50

60

70

80

90

0 5 10 15 20 25 30 35

% Saturation

Drying Cycle Number


Run 1

Run 2

Run 3

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Drying of CLEO as ppm Water (All drying cycles)

Drying of CLEO as ppm Water (Drying 15‐35)

The data above shows that CLEO meets the acceptance criteria laid out in ISO 13628‐6 as the

water content is reduced from >80% saturation to <30% saturation within the 35 cycle limit.

0

500

1000

1500

2000

2500

3000

0 5 10 15 20 25 30 35

Water Content / ppm

Number of Cycles


Run 1

Run 2

Run 3

0

50

100

150

200

250

300

350

400

450

500

15 17 19 21 23 25 27 29 31 33 35

Water Content/ ppm

Number of Cycles


Run 1

Run 2

Run 3

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4.3.5 – Water Absorption Test


The purpose of this test is to measure the capability of the oil to absorb water (i.e. the blotter

paper functionality). The test oil is carefully added to artificial seawater and then stirred. The %

saturation of the oil is measured over time until 80% saturation is achieved.

Procedure

This test should be carried out at 20°C. Add 40 grams of artificial seawater (20% w/w) to a 400ml

tall form glass beaker. Carefully add 200 grams of dry test oil (≤ 20% saturation at 20°C). Place a

magnetic follower in the water phase. Use an overhead stirrer to stir the oil phase. Place the

paddle of the overhead stirrer in the middle of the oil phase. Set the overhead stirrer speed such

that the oil / water interface is not broken and there is no vortex generated. Set the speed of the

magnetic follower such that the water phase is gently moved around but the interface is not

broken. This may be as little as 100rpm. The stirring is designed to gently move the oil over the

water phase and continually move it past the moisture sensor. Place the moisture sensor so that it

is in the middle of the oil phase. Record the % saturation at time intervals, for example every 15

minutes, until the oil reaches 80% saturation.

ACCEPTANCE CRITERIA

There are no acceptance criteria for this test.

RESULTS

The results for water absorption test for CLEO and Sea water are tabulated below and in the

graph overleaf.

Time Mins % Saturation

0 28.4

30 50.1

60 66.3

120 76.1

180 84.9

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Plot of % saturation as a function of time for CLEO and Sea Water

20

30

40

50

60

70

80

90

0 20 40 60 80 100 120 140 160 180 200

% Saturation

Time / Minutes

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4.4 – Control Fluid Compatibility


The primary fluid is mixed with Transaqua HT2, Transaqua HC10, Oceanic HW443, Brayco

Micronic SV/3, Brayco Micronic SV/3, Pelagic 100 and Pelagic 100 HC in specified mixing ratio at

ambient and moderate temperatures for 4 weeks. The following methods are used to assess the

mixtures:‐

Visual inspection

Viscosity

Pour point.

PROCEDURE

The primary fluid is mixed with the control fluid in the mixing ratios of 90:10; 75:25; 50:50; 25:75

and 10:90 % v/v. The samples are exposed undisturbed at 5, 20 and 70 °C for 4 weeks and the

appearance is observed.

ACCEPTANCE CRITERIA

The acceptance criteria are as follows.

No change in appearance except natural colour changes if the fluids are of different

colours, at any mixing ratio.

No separation at any mixing ratios.

Viscosity of any mixing ratio should not increase by more than 20% after 4 wks.

Pour point of all mixing ratios to be less than ‐30 °C (when mixing oil fluids).

RESULTS

Results for each fluid mixture with CLEO are outlined below. Results are broadly as expected

when mixing with water based control fluids. CLEO is fully compatible with Brayco Micronic SV/B

and SV/3.

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Page Intentionally Left Blank.

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4.4.1.a – CLEO Compatibility with Pelagic 100 @ 5 °C

% v/v CLEO : % v/v

Pelagic 100

Aging Time / weeks

Appearance Change in appearance vs. initial mixture

(separation, solids etc.)

90:10 N/A Two phases. Top colourless and hazy. Bottom

colourless, clear &bright. N/A

75:25 N/A Two phases. Top colourless and opaque. Bottom

colourless, clear & bright. N/A

50:50 N/A Two phases. Top colourless and opaque. Bottom is

colourless, hazy (semi‐translucent). N/A


colourless, hazy (semi‐translucent). N/A


colourless, slightly hazy. N/A

90:10 1 Two phases. Top trace hazy colourless. Bottom

colourless, clear and bright. There is aeration at the interface.

Top phase has become clearer. Aeration is seen at the interface.

75:25 1 Two phases. Top is colourless and trace hazy. Bottom is colourless, clear and bright. There is aeration at the

interface.

Top phase has become clearer. Aeration is seen at the interface.

50:50 1 Two phases. Top colourless, clear and bright with

foam‐like aeration around upper surface. Interface is foamy. Lower layer is slightly hazy.

Both phases clearer. Foam‐like aeration seen in upper phase and interface.

25:75 1 Two phases. Top colourless, clear and bright with

foam‐like aeration around upper surface. Interface is foamy. Lower layer is slightly hazy.

Both phases clearer. Foam‐like aeration seen in upper phase and interface.

10:90 1 Two phases. Top is clear and bright with foam‐like aeration. Lower layer is colourless and slightly hazy.

Top phase has become clearer. Aeration seen in upper phase.

90:10 2 Two phases. Top is colourless clear and bright. Bottom is colourless, clear and bright. There is aeration at the

interface. Top phase has become clearer



50:50 2 Two phases. Top is colourless clear and bright. Bottom

is colourless, trace hazy. There is a large aerated interface.

Both phases have become clearer.


interface. Both phases have become clearer.

10:90 2 Two phases. Top is clearing from the top and is colourless. Bottom is colourless, clear and bright.


90:10 3 Two phases, both clear and bright with aeration at








10:90 3 Two phases. Top is clearing from the top and is colourless. Bottom is colourless, clear and bright.












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35

CLEO Compatibility with Pelagic 100 @ 5 °C

Time 90% CLEO : 10% Pelagic

100

75% CLEO : 25% Pelagic

100


100

25% CLEO : 75 % Pelagic 100


100

Initial

1 week

2 week

3 week

4 week

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4.4.1.b – CLEO Compatibility with Pelagic 100 @ 20 °C

% v/v CLEO : % v/v Pelagic

100

Aging Time / weeks



90:10 1 Two phases. Top colourless and hazy. Bottom colourless,

clear and bright. Aeration at interface. Aeration at the interface.

75:25 1 Two phases. Top colourless and hazy. Bottom colourless,

clear and bright. Aeration at interface. Aeration at the interface.

50:50 1 Two phases. Top opaque, white & clearing from the top.

Bottom colourless, clear and bright. Upper layer is beginning to clear.

25:75 1 Two phases. Top very pale yellow and slightly hazy. Bottom

colourless and trace hazy. Both phases have become clearer.

10:90 1 Two phases. Top very pale yellow and slightly hazy. Bottom

colourless, clear and bright. Both phases have become clearer.

90:10 2 Both phases colourless clear and bright with aeration at the






25:75 2 Two phases. Top colourless, clear and bright. Bottom

colourless, trace hazy. Both phases have become clearer.



90:10 3 Two phases, top colourless and hazy, bottom colourless

clear and bright with aeration at interface. Both phases have become clearer.






colourless, trace hazy. Both phases have become clearer.



90:10 4 Two phases, top colourless and slightly hazy, bottom colourless clear and bright with aeration at interface.


75:25 4 Two phases, top colourless and slightly hazy, bottom colourless clear and bright with aeration at interface.


50:50 4 Two phases, top colourless and slightly hazy, bottom

colourless trace hazy. Both phases have become clearer.





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100


100


100



100

Initial

1 week

2 week

3 week

4 week

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38

4.4.1.c – CLEO Compatibility with Pelagic 100 @ 70 °C

% v/v CLEO : % v/v Pelagic 100

Aging Time / weeks



90:10 1 Two phases. Both colourless clear and bright. The upper

layer becomes hazy on cooling. Both phases have become clearer.


layer becomes hazy on cooling Both phases have become clearer.





































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100


100


100



100

Initial

1 week

2 week

3 week

4 week

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4.4.2.a – CLEO Compatibility with Transaqua HT‐2 @ 5 °C

% v/v CLEO : % v/v

Transaqua HT‐2

Aging Time / weeks

Appearance Change in appearance vs. initial mixture (separation, solids etc.)

90:10 N/A Two phases, top opaque white. Bottom pale yellow and hazy. N/A

75:25 N/A Two phases, top opaque white. Bottom pale yellow and hazy N/A




90:10 1 Two phases both clear and bright Both layers have become clear

75:25 1 Two phases both clear and bright Both layers have become clear

50:50 1 Two phases, top opaque white. Bottom pale yellow clear and bright. Bottom layer has become clear



90:10 2 Two phases. Top colourless clear and bright. Bottom yellow, clear

and bright. Both layers have become clear

75:25 2 Two phases. Top colourless clear and bright. Bottom yellow, clear

and bright. Both layers have become clear

50:50 2 Two phases. Top opaque white and aerated, clearing from the top.

Bottom pale yellow clear and bright. Both layers have become clear


Bottom pale yellow clear and bright. Bottom layer has become clearer


Bottom pale yellow clear and bright. Bottom layer has become clear

90:10 3 Two clear and bright phases. Top colourless, bottom yellow.

Aeration at interface. Both layers have become clear



















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41

CLEO Compatibility with Transaqua HT‐2 @ 5 °C

Time

90% CLEO : 10%

Transaqua HT‐2

75% CLEO : 25%

Transaqua HT‐2

50% CLEO : 50%

Transaqua HT‐2

25% CLEO : 75 % Transaqua

HT‐2

10% CLEO : 90%

Transaqua HT‐2

Initial

1 week

2 week

3 week

4 week

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4.4.2.b – CLEO Compatibility with Transaqua HT‐2 @ 20 °C

% v/v CLEO : % v/v

Transaqua HT‐2

Aging Time / weeks


90:10 1 Two phases. Top colourless and slightly hazy. Bottom clear and

bright. Bottom layer has become clear. Top

has almost become clear.

75:25 1 Two phases. Top colourless and slightly hazy. Bottom clear and


has almost become clear.

50:50 1 Two phases. Top white and opaque. Bottom clear and bright. Bottom layer has become clear



90:10 2 Two phases. Top colourless slightly hazy. Bottom yellow, clear

and bright. Aeration seen at interface. Top layer has become clearer

75:25 2 Two phases. Top colourless slightly hazy. Bottom yellow, clear

and bright. Aeration seen at interface. Top layer has become clearer

50:50 2 Two phases. Top colourless and opaque. Bottom pale yellow,

clear and bright. Bottom layer has become clear

25:75 2 Two phases. Top colourless and opaque, clearing from the top.

Bottom pale yellow, clear and bright. Both layers have become clearer.

10:90 2 Two phases. Top colourless clear and bright with aeration at

interface. Bottom yellow, clear and bright. Both layers have become clearer.

90:10 3 Two phases. Top hazy colourless. Bottom yellow, clear and bright.

Aeration seen at interface. Top layer has become clearer

75:25 3 Two phases. Top hazy colourless. Bottom yellow, clear and bright.

Aeration seen at interface. Top layer has become clearer

50:50 3 Two phases. Top white opaque. Bottom yellow, clear and bright.

Aeration seen at interface. Bottom layer has become clear

25:75 3 Two phases. Top is a white opaque. Bottom is yellow, clear and

bright. Aeration seen at interface. Bottom layer has become clear

10:90 3 Two phases. Top slightly hazy colourless. Bottom yellow, clear

and bright. Aeration seen at interface. Both layers have become clearer.

90:10 4 Two phases both clear and bright, top is colourless, bottom is

pale yellow. Both layers have become clearer.

75:25 4 Two phases both clear and bright, top is colourless, bottom is

pale yellow. Both layers have become clearer.

50:50 4 Two phases. Top white opaque. Bottom yellow, clear and bright.

Aeration seen at interface. Bottom layer has become clear

25:75 4 Two phases. Top is a white opaque. Bottom is yellow, clear and

bright. Aeration seen at interface. Bottom layer has become clear

10:90 4 Two phases. Top trace hazy colourless. Bottom yellow, clear and

bright. Aeration seen at interface. Both layers have become clearer.

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Time

90% CLEO : 10%

Transaqua HT‐2

75% CLEO : 25%

Transaqua HT‐2

50% CLEO : 50%

Transaqua HT‐2


HT‐2

10% CLEO : 90%

Transaqua HT‐2

Initial

1 week

2 week

3 week

4 week

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4.4.2.c – CLEO Compatibility with Transaqua HT‐2 @ 70 °C

% v/v CLEO : % v/v

Transaqua HT‐2

Aging Time / weeks


90:10 1 Two phases. Top colourless and hazy. Bottom clear and bright.

The upper layer becomes hazy on cooling Bottom layer has become clear. Top

layer has become clearer.

75:25 1 Two phases. Top colourless and hazy. Bottom clear and bright.

The upper layer becomes hazy on cooling Bottom layer has become clear. Top

has layer become clearer.

50:50 1 Two phases. Top colourless and hazy. Bottom is clear and bright. Hazy interlayer seen. The upper layer becomes hazy on cooling

Bottom layer has become clear. Top has layer become clearer.

Hazy interlayer seen

25:75 1 Two phases. Top colourless and hazy. Bottom is clear and bright. Hazy interlayer seen. The upper layer becomes hazy on cooling



10:90 1 Two phases. Top hazy and clearing from the top downwards. Bottom is yellow clear and bright. Hazy interlayer seen. The

upper layer becomes hazy on cooling



90:10 2 Two phases. Top colourless, clear and bright, going hazy on

cooling. Bottom yellow, clear and bright. Both layers have become clearer.

75:25 2 Two phases. Top is colourless, clear and bright, going hazy on

cooling. Bottom is yellow, clear and bright. Both layers have become clearer.

50:50 2 Two phases. Top is clearing from top to be colourless, clear and bright to white and opaque, but goes hazy on cooling. Hazy

Interlayer seen. Bottom is yellow, clear and bright.

Both layers have become clearer. Hazy interlayer seen.

25:75 2 Two phases. Top is clearing from top to be colourless, clear and bright to white and opaque but goes hazy on cooling. Hazy



10:90 2 Two phases. Top is clearing from top to be colourless, clear and bright to white and opaque but goes hazy on cooling. Hazy



90:10 3 Two phases. Top is colourless, clear and bright but goes hazy on




50:50 3 Two phases. Top is clearing from top to be colourless, clear and bright with white and opaque interlayer but goes hazy on cooling.

Bottom is yellow, clear and bright with aeration at interface

Both layers have become clearer. Hazy interlayer seen





cooling. Bottom is yellow, clear and bright Both layers have become clearer. Hazy

interlayer seen













cooling. Bottom is yellow, clear and bright Both layers have become clearer. Hazy

interlayer seen

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Time

90% CLEO : 10%

Transaqua HT‐2

75% CLEO : 25%

Transaqua HT‐2

50% CLEO : 50%

Transaqua HT‐2


HT‐2

10% CLEO : 90%

Transaqua HT‐2

Initial

1 week

2 week

3 week

4 week

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4.4.3.a – CLEO Compatibility with Oceanic HW443 @ 5 °C

% v/v CLEO : % v/v Oceanic HW443

Aging Time / weeks



90:10 N/A Two phases seen. Top phase is hazy with some droplets

of HW443. Bottom phase is clear and bright. N/A

75:25 N/A Two phases. Top is hazy. Bottom is clear and bright. Droplets of lower phase are present in the upper

phase. N/A

50:50 N/A Two phases. Top is hazy, semi‐translucent. Bottom is trace hazy. Droplets of lower phase are present in the

upper phase. N/A

25:75 N/A Two phases. Top is slightly hazy. Bottom is slightly hazy.

Droplets of lower phase are present in the upper phase.

N/A

10:90 N/A Two phases. Top is clearing from top to bottom.

Bottom is slightly hazy N/A

90:10 1 Two phases. Top is colourless, clear and bright. Bottom

is yellow clear and bright. Top layer has cleared.




is yellow trace hazy. Top layer has cleared.
















is dark yellow, clear and bright. Both layers have cleared.




is dark yellow, clear and bright. Slight aeration at interface

Both layers have cleared.

25:75 3 Two phases, both clear and bright. Top is pale yellow,bottom is dark yellow. Slight aeration at interface


10:90 3 Two phases. Top is yellow, clear and bright. Bottom is

dark yellow, clear and bright. Both layers have cleared.






is dark yellow, clear and bright. Slight aeration at interface


25:75 4 Two phases, both clear and bright. Top is pale yellow, bottom is dark yellow. Slight aeration at interface


10:90 4 Two phases. Top is yellow, clear and bright. Bottom is

dark yellow, clear and bright. Both layers have cleared.

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CLEO Compatibility with Oceanic HW443 @ 5 °C

Time 90% CLEO : 10% Oceanic

HW443

75% CLEO : 25% Oceanic

HW443


HW443

25% CLEO : 75 % Oceanic HW443


HW443

Initial

1 week

2 week

3 week

4 week

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4.4.3.b – CLEO Compatibility with Oceanic HW443 @ 20 °C


Aging Time / weeks



90:10 1 Two phases. Top is slightly hazy and colourless, Bottom

is yellow, clear and bright. Top layer has partially cleared.




is slightly hazy and yellow. Top layer has partially cleared.



































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HW443


HW443


HW443



HW443

Initial

1 week

2 week

3 week

4 week

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4.4.3.c – CLEO Compatibility with Oceanic HW443 @ 70 °C


Aging Time / weeks



90:10 1 Two phases. Top is hazy, semi‐translucent. Bottom is

clear and bright. Droplets of bottom layer in top layer

have gone.


clear and bright. Droplets of bottom layer in top layer

have gone.


clear and bright.

Bottom layer has become clear.Droplets of bottom layer in top layer

have gone.


clear and bright.

Top layer has become hazier, bottom layer has become clear.

Droplets of bottom layer in top layer have gone.

10:90 1 Two phases. Top is slightly hazy. Bottom is clear and


layer has become clearer.

90:10 2 Two phases. Top is colourless, clear and bright, going hazy on cooling. Bottom is orange, clear and bright.

Top phase has become clearer.




Both layers have become clearer.

25:75 2 Two phases. Top is pale yellow, slightly hazy, going hazy

on cooling. Bottom is orange, clear and bright. Bottom layer has become clearer.

10:90 2 Two phases. Top is pale yellow, slightly hazy, going hazy

on cooling. Bottom is orange, clear and bright. Both layers have become clearer.





50:50 3 Two phases. Top is pale yellow, clear and bright, going hazy on cooling. Bottom is orange, clear and bright.


25:75 3 Two phases. Top is pale yellow, trace hazy, going hazy

on cooling. Bottom is orange, clear and bright. Top phase has become clearer.







50:50 4 Two phases. Top is pale yellow, clear and bright, going hazy on cooling. Bottom is orange, clear and bright.






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51



HW443


HW443


HW443



HW443

Initial

1 week

2 week

3 week

4 week

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4.4.4.a – CLEO Compatibility with Transaqua HC‐10 @ 5 °C

% v/v CLEO : % v/v Transaqua HC‐10

Aging Time / weeks



90:10 N/A Two phases. Top is colourless, hazy. Bottom is yellow

clear and bright. N/A

75:25 N/A Two phases. Top is colourless, hazy. Bottom is yellow


50:50 N/A Two phases. Top is colourless and opaque. Bottom is

yellow and slightly hazy. N/A


yellow and hazy N/A


yellow and slightly hazy. N/A

90:10 1 Two phases, both clear and bright. Top is colourless, bottom is yellow. Aeration is seen at the interface.

Top layer has become clearer. Aeration is seen at the interface.



50:50 1 Two phases. Top is white and opaque. Bottom is yellow

and slightly hazy. No changes


and slightly hazy. Bottom layer has become clearer.


and trace hazy. Bottom layer has become clearer.





50:50 2 Two phases. Top is clearing from top, but mainly white

and opaque. Bottom is yellow and slightly hazy. No changes

25:75 2 Two phases. Top is colourless, opaque and aerated.

Bottom is pale yellow and slightly hazy. Bottom layer has become clearer.

10:90 2 Two phases. Top is colourless and opaque. Bottom is

pale yellow, clear and bright. Bottom layer has become clearer.





















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CLEO Compatibility with Transaqua HC‐10 @ 5 °C

Time

90% CLEO : 10%

Transaqua HC‐10

75% CLEO : 25%

Transaqua HC‐10

50% CLEO : 50%

Transaqua HC‐10


HC‐10

10% CLEO : 90%

Transaqua HC‐10

Initial

1 week

2 week

3 week

4 week

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4.4.4.b – CLEO Compatibility with Transaqua HC‐10 @ 20 °C


Aging Time / weeks



90:10 1 Two phases. Top is colourless, hazy. Bottom is yellow

clear and bright. No changes

75:25 1 Two phases. Top is colourless, hazy. Bottom is yellow clear and bright. Aeration is seen at the interface.

Aeration is seen at the interface.

50:50 1 Two phases. Top is white and opaque. Bottom is

yellow, clear and bright. Bottom layer has become clearer.

25:75 1 Two phases. Top is white and opaque and clearing from

the top. Bottom is yellow, clear and bright. Both layers are becoming clearer.

10:90 1 Two phases. Top is white and opaque and clearing from

the top. Bottom is yellow, clear and bright. Both layers are becoming clearer.

90:10 2 Two phases, both clear and bright. Top is colourless,

bottom is pale yellow. Top layer has become clearer.

75:25 2 Two phases, both clear and bright. Top is colourless,

bottom is pale yellow. Aeration is seen at the interface. Top layer has become clearer.


pale yellow, clear and bright. Aeration seen at interface Aeration is seen at the interface.





90:10 3 Two phases, top is colourless and slightly hazy, bottom

is pale yellow, clear and bright. Top layer is clearing.









90:10 4 Two phases, top is colourless and trace hazy, bottom is

pale yellow, clear and bright. Top layer is clearing.

75:25 4 Two phases, top is colourless and trace hazy, bottom is

pale yellow, clear and bright. Top layer is clearing.


is pale yellow, clear and bright. Aeration seen at interface.

Top layer is clearing.





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Time

90% CLEO : 10%

Transaqua HC‐10

75% CLEO : 25%

Transaqua HC‐10

50% CLEO : 50%

Transaqua HC‐10


HC‐10

10% CLEO : 90%

Transaqua HC‐10

Initial

1 week

2 week

3 week

4 week

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4.4.4.c – CLEO Compatibility with Transaqua HC‐10 @ 70 °C


Aging Time / weeks



90:10 1 Two phases both clear and bright. Top is colourless, bottom is yellow. Top layer becomes hazy on cooling.

Both layers have become clear and bright.





25:75 1 Two phases. Top is colourless with aeration at the

interface. Bottom is yellow, clear and bright. Top layer becomes hazy on slight cooling.

Both layers have become clearer. Aeration is seen at the interface.

10:90 1 Two phases. Top is colourless with aeration at the

interface. Bottom is yellow, clear and bright. Top layer becomes hazy on slight cooling.

Both layers have become clearer. Aeration is seen at the interface.

90:10 2 Two phases. Top is colourless, clear and bright going hazy on cooling. Bottom is yellow, clear and bright.

Top layer has become clearer.





25:75 2 Two phases. Top is colourless, clear and bright going hazy on cooling. Bottom is yellow, clear and bright. An

aerated interface has formed.

Both layers have become clearer. An interface has formed




























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Time

90% CLEO : 10%

Transaqua HC‐10

75% CLEO : 25%

Transaqua HC‐10

50% CLEO : 50%

Transaqua HC‐10


HC‐10

10% CLEO : 90%

Transaqua HC‐10

Initial

1 week

2 week

3 week

4 week

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4.4.5.a – CLEO Compatibility with Brayco Micronic SV/B @ 5 °C

% v/v CLEO : % v/v Brayco Micronic SV/B

Aging Time / weeks



90:10 N/A Single phase clear and bright. N/A





90:10 1 Single phase clear and bright. No changes





















Initial Viscosity @ 40 °C Viscosity @ 40 °C after 4 weeks

aging % Change in Viscosity

90:10 8.38 8.16 2.6

75:25 8.04 7.98 0.8

50:50 8.16 7.96 2.5

25:75 8.22 7.92 3.6

10:90 8.47 7.86 7.2


Initial Pour Point / °C * Pour Point after 4 weeks aging

* ISO 13628‐6

90:10 <‐30 °C <‐30 °C Pass

75:25 <‐30 °C <‐30 °C Pass

50:50 <‐30 °C <‐30 °C Pass

25:75 <‐30 °C <‐30 °C Pass

10:90 <‐30 °C <‐30 °C Pass

* Mixtures were stable at ‐32 °C overnight.

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CLEO Compatibility with Brayco Micronic SV/B @ 5 °C

Time

90% CLEO : 10% Brayco Micronic SV/B

75% CLEO:25% Brayco Micronic SV/B



10% CLEO : 90% : Brayco Micronic SV/B

Initial

1 week

2 week

3 week

4 week

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4.4.5.b – CLEO Compatibility with Brayco Micronic SV/B @ 20 °C


Aging Time / weeks


























90:10 8.38 8.01 4.4

75:25 8.04 8.26 2.7

50:50 8.16 7.83 4.0

25:75 8.22 7.98 2.9

10:90 8.47 8.26 2.5



* ISO 13628‐6

90:10 <‐30 °C <‐30 °C Pass

75:25 <‐30 °C <‐30 °C Pass

50:50 <‐30 °C <‐30 °C Pass

25:75 <‐30 °C <‐30 °C Pass

10:90 <‐30 °C <‐30 °C Pass


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Time






Initial

1 week

2 week

3 week

4 week

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4.4.5.c – CLEO Compatibility with Brayco Micronic SV/B @ 70 °C


Aging Time / weeks


























90:10 8.38 8.10 3.3

75:25 8.04 7.73 3.9

50:50 8.16 7.86 3.7

25:75 8.22 8.01 2.6

10:90 8.47 8.04 5.1



* ISO 13628‐6

90:10 <‐30 °C <‐30 °C Pass

75:25 <‐30 °C <‐30 °C Pass

50:50 <‐30 °C <‐30 °C Pass

25:75 <‐30 °C <‐30 °C Pass

10:90 <‐30 °C <‐30 °C Pass


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Time






Initial

1 week

2 week

3 week

4 week

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ISO 13628‐6 (2012)

64

4.4.6.a – CLEO Compatibility with Pelagic 100HC @ 5 °C

% v/v CLEO : % v/v Pelagic 100HC

Aging Time / weeks



90:10 N/A Two phases. Top is colourless, hazy. Bottom is pink,



pink and slightly hazy. N/A

50:50 N/A Separating into 2 phases, both are opaque. N/A

25:75 N/A Single phase beginning to separate into two phases.

Pink and opaque. N/A

10:90 N/A Single phase beginning to separate into two phases.

Pink and opaque. N/A


is pink clear and bright. Aeration is seen at the interface.

Upper phase has become clear. Aeration is seen at the interface.



Both phases have become clearer. Aeration is seen at the interface.

50:50 1 Two phases. Top is opaque and still holding some pink

colouration. Bottom is pink and hazy. Both phases have become clearer


is pink and hazy. Both phases have become clearer




is pink clear and bright. Both phases have become clearer




50:50 2 Two phases. Top is clearing from the top, colourless, clear and bright to opaque pink. Bottom is pink and

hazy. Both phases have become clearer













is pink and slightly hazy. Both phases have become clearer














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65

CLEO Compatibility with Pelagic 100HC @ 5 °C


100HC

75% CLEO: 25% Pelagic

100HC


100HC


100HC


100HC

Initial

1 week

2 week

3 week

4 week

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66

4.4.6.b – CLEO Compatibility with Pelagic 100HC @ 20 °C


Aging Time / weeks



90:10 1 Two phases. Top is colourless and hazy. Bottom is pink,

clear and bright. No changes

75:25 1 Two phases. Top is colourless and hazy. Bottom is pink,

clear and bright. Bottom phase has become clearer.

50:50 1 Two phases. Top is colourless and slightly hazy. Bottom

is pink, clear and bright. Bottom phase has become clearer.

25:75 1 Two phases. Top is colourless and slightly hazy. Bottom

is pink, clear and bright. Bottom phase has become clearer.

10:90 1 Two phases. Top is colourless and trace hazy. Bottom is

pink, clear and bright. Bottom phase has become clearer.

90:10 2 Two phases both clear and bright. Top is colourless,

bottom is pink. Both phases have become clearer.

75:25 2 Two phases both clear and bright. Top is colourless, bottom is pink. There is a slight aerated interface.




























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100HC


100HC


100HC


100HC


100HC

Initial

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2 week

3 week

4 week

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68

4.4.6.c – CLEO Compatibility with Pelagic 100HC @ 70 °C


Aging Time / weeks



90:10 1 Two phases both clear and bright. Top is colourless,bottom is pink. The top phase goes hazy on cooling.


75:25 1 Two phases both clear and bright. Top is colourless, bottom is pink. The top phase goes hazy on cooling.






































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100HC


100HC


100HC


100HC


100HC

Initial

1 week

2 week

3 week

4 week

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70

4.4.7.a – CLEO Compatibility with Brayco Micronic SV/3 @ 5 °C

% v/v CLEO : % v/v Brayco Micronic SV/3

Aging Time / weeks


90:10 1 Single phase, very pale yellow fluid. No visible change.

75:25 1 Single phase, pale yellow fluid. No visible change.


25:75 1 Single phase, yellow fluid. No visible change.

10:90 1 Single phase yellow fluid. No visible change.

















Initial Viscosity @ 40 °C / cSt Viscosity @ 40 °C after 4 weeks

aging / cSt Change in Viscosity

90:10 8.59 8.44 1.7 %

75:25 8.90 8.90 0 %

50:50 9.51 9.51 0 %

25:75 10.37 10.07 1.9 %

10:90 10.65 10.62 0.3 %



* ISO 13628‐6

90:10 <‐30 °C <‐30 °C Pass

75:25 <‐30 °C <‐30 °C Pass

50:50 <‐30 °C <‐30 °C Pass

25:75 <‐30 °C <‐30 °C Pass

10:90 <‐30 °C <‐30 °C Pass


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71

CLEO Compatibility with Brayco Micronic SV/3 @ 5 °C

Time 90% CLEO : 10% Brayco

Micronic SV/3

75% CLEO: 25% Brayco

Micronic SV/3

50% CLEO : 50% Brayco

Micronic SV/3


Micronic SV/3


Micronic SV/3

Initial

1 week

2 week

3 week

4 week

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4.4.7.b – CLEO Compatibility with Brayco Micronic SV/3 @ 20 °C


Aging Time / weeks








90:10 2 Single phase, pale yellow liquid Slight darkening from Brayco SV/3.

75:25 2 Single phase yellow liquid Slight darkening from Brayco SV/3.

















90:10 8.59 8.32 3.1 %

75:25 8.90 8.84 0.7 %

50:50 9.51 9.51 0 %

25:75 10.37 9.94 4.4 %

10:90 10.65 10.59 0.6 %



* ISO 13628‐6

90:10 <‐30 °C <‐30 °C Pass

75:25 <‐30 °C <‐30 °C Pass

50:50 <‐30 °C <‐30 °C Pass

25:75 <‐30 °C <‐30 °C Pass

10:90 <‐30 °C <‐30 °C Pass


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Micronic SV/3


Micronic SV/3


Micronic SV/3


Micronic SV/3


Micronic SV/3

Initial

1 week

2 week

3 week

4 week

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74

4.4.7.c – CLEO Compatibility with Brayco Micronic SV/3 @ 70 °C


Aging Time / weeks


























90:10 8.59 8.47 1.4 %

75:25 8.90 8.81 0.1 %

50:50 9.51 9.48 0.3 %

25:75 10.37 10.21 1.5 %

10:90 10.65 10.68 0.3 %



* ISO 13628‐6

90:10 <‐30 °C <‐30 °C Pass

75:25 <‐30 °C <‐30 °C Pass

50:50 <‐30 °C <‐30 °C Pass

25:75 <‐30 °C <‐30 °C Pass

10:90 <‐30 °C <‐30 °C Pass


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Micronic SV/3


Micronic SV/3


Micronic SV/3


Micronic SV/3


Micronic SV/3

Initial

1 week

2 week

3 week

4 week

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76

4.5 – Completion Fluid Compatibility

METHODS AND MEASUREMENTS:

The control fluid is mixed with specific completion fluids in defined mixing ratios at 5 and 20 °C.

PROCEDURE

The control fluid is mixed with the following completion fluids in the volume mixing ratios:

99.5:0.5, 99:1, 98:2, 95:5, and 90:10 (mixing ratios are defined as control fluid : contaminant) (%

completion fluid) mixing ratios:

Calcium chloride (CaCl2), calcium bromide (CaBr2), zinc bromide (ZnBr2), zinc chloride (ZnCl2),

potassium formate (K‐formate) and caesium formate (Cs‐formate). The actual brines shall be

selected from commercially available products, and the type, brand and other relevant data shall

be included in the report.

The samples are exposed at 5 and 20 °C for 4 weeks. The mixtures are shaken vigorously on

mixing and on intervals (1, 7, 14 and 21 days). The appearance of the mixtures and formation of

separations are observed instantly after being shaken, after 1 hour, 1 day, 1 week and 4 weeks.

ACCEPTANCE CRITERIA

There are no general acceptance criteria related to this property. The results have to be evaluated

for the individual projects for which they are relevant. It is up to each specific project to define

project‐related criteria if this is considered necessary.

RESULTS

Results for each fluid mixture with CLEO are outlined below. Results are broadly as expected

when mixing with water based control fluids.

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78

4.5.1.a – CLEO Compatibility with Calcium Chloride Brine 11.2 ppg (Lab Made) @ 5 °C

% v/v CLEO : % v/v CaCl2 Brine 11.2ppg

Aging Time Appearance before shaking Appearance after shaking

99.5 : 0.5 N/A Two phases, both colourless clear and bright. Two clear & bright phases, brine bubbles in oil phase.

99 : 1 N/A Two phases, both colourless clear and bright. Two clear & bright phases, brine bubbles in oil phase.




99.5 : 0.5 1 hour Two phases, both colourless clear and bright. Two clear & bright phases, brine bubbles in oil phase.

99 : 1 1 hour Two phases, both colourless clear and bright. Two clear & bright phases, brine bubbles in oil phase.




99.5 : 0.5 1 day Two phases, both colourless clear and bright. Two clear & bright phases, brine bubbles in oil phase.

99 : 1 1 day Two phases, both colourless clear and bright. Two clear & bright phases, brine bubbles in oil phase.




99.5 : 0.5 1 week Two phases, both colourless clear and bright. Two clear & bright phases, brine bubbles in oil phase.

99 : 1 1 week Two phases, both colourless clear and bright. Two clear & bright phases, brine bubbles in oil phase.




99.5 : 0.5 2 weeks Two phases, both colourless clear and bright. Two clear & bright phases, brine bubbles in oil phase.

99 : 1 2 weeks Two phases, both colourless clear and bright. Two clear & bright phases, brine bubbles in oil phase.




99.5 : 0.5 3 weeks Two phases, both colourless clear and bright. Top phase clear and bright, bottom phase trace hazy

with some brine bubbles visible in oil phase.

99 : 1 3 weeks Two phases, both colourless clear and bright. Top phase clear and bright, bottom phase trace hazy








99.5 : 0.5 4 weeks Two phases, trace hazy top phase with a clear

and bright bottom phase. Mixture not shaken after 4 weeks in line with testing

protocol.

99 : 1 4 weeks Two phases, trace hazy top phase with a clear


protocol.



protocol.



protocol.



protocol.

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79

CLEO compatibility with Calcium Chloride Brine@ 5 °C – Lab Made 11.2 ppg

Aging Time

Before Shaking After Shaking

99.5 % CLEO : 0.5% CaCl2 Brine

99% CLEO : 1% CaCl2 Brine


95% CLEO: 5% CaCl2 Brine







1 day

1 week

2 week

3 week

4 week Mixture not shaken after 4 weeks in line with testing

protocol.

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80

4.5.1.b – CLEO Compatibility with Calcium Chloride Brine 11.2 ppg (Lab Made) @ 20 °C

% v/v CLEO : % v/v CaCl2 Brine 11.2ppg
































99.5 : 0.5 4 weeks Two phases, both colourless clear and bright. Mixture not shaken after 4 weeks in line with testing

protocol.

99 : 1 4 weeks Two phases, both colourless clear and bright. Mixture not shaken after 4 weeks in line with testing

protocol.


protocol.


protocol.


protocol.

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81

CLEO Compatibility with Calcium Chloride Brine 11.2 ppg (Lab Made) at 20 °C

Aging Time












1 day

1 week

2 week

3 week


protocol.

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82

4.5.2.a – CLEO Compatibility with Calcium Bromide Brine 12.5 ppg (Lab Made) @ 5 °C

% v/v CLEO : % v/v CaBr2 Brine 12.5

ppg
































99.5 : 0.5 4 weeks Two phases, both trace hazy. Mixture not shaken after 4 weeks in line with testing

protocol.

99 : 1 4 weeks Two phases, both trace hazy. Mixture not shaken after 4 weeks in line with testing

protocol.


protocol.


protocol.


protocol.

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83

CLEO compatibility with Calcium Bromide Brine @ 5°C – Lab Made 12.5 ppg

Aging Time


99.5 % CLEO : 0.5% CaBr2 Brine

99% CLEO :

1% CaBr2 Brine

98% CLEO :

2% CaBr2 Brine

95% CLEO: 5% CaBr2 Brine

90% CLEO : 10% CaBr2 Brine


99% CLEO :

1% CaBr2 Brine

98% CLEO :

2% CaBr2 Brine



1 day

1 week

2 week

3 week


protocol.

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ISO 13628‐6 (2012)

84

4.5.2.b – CLEO Compatibility with Calcium Bromide Brine 12.5 ppg (Lab Made) @ 20 °C

% v/v CLEO : % v/v CaBr2 Brine 12.5

ppg

































protocol.


protocol.


protocol.


protocol.


protocol.

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85

CLEO Compatibility with Calcium Bromide Brine 12.5 ppg (Lab Made) @ 20 °C

Aging Time



99% CLEO :

1% CaBr2 Brine

98% CLEO :

2% CaBr2 Brine




99% CLEO :

1% CaBr2 Brine

98% CLEO :

2% CaBr2 Brine



1 day

1 week

2 week

3 week


protocol.

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86

4.5.3.a – CLEO Compatibility with Zinc Bromide Brine 19.2 ppg (Lab Made) @ 5 °C

% v/v CLEO : % v/v ZnBr2

Brine 19.2ppg Aging Time Appearance before shaking Appearance after shaking


























99.5 : 0.5 3 weeks Two phases, both clear and bright. Top layer

pale pink Two clear & bright phases, brine bubbles in oil phase.

99 : 1 3 weeks Two phases, both clear and bright. Top layer








99.5 : 0.5 4 weeks Two phases, trace hazy pale pink tinted top phase with a clear and bright bottom phase.

Mixture not shaken after 4 weeks in line with testing protocol.

99 : 1 4 weeks Two phases, trace hazy pale pink tinted top phase with a clear and bright bottom phase.








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87

CLEO Compatibility with Zinc Bromide Brine 19.2 ppg (Lab Made) @ 5 °C

Aging Time


99.5 % CLEO : 0.5% ZnBr2 Brine

99% CLEO :

1% ZnBr2 Brine

98% CLEO :

2% ZnBr2 Brine

95% CLEO: 5% ZnBr2 Brine

90% CLEO : 10% ZnBr2 Brine


99% CLEO :

1% ZnBr2 Brine

98% CLEO :

2% ZnBr2 Brine



1 day

1 week

2 week

3 week


protocol.

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ISO 13628‐6 (2012)

88

4.5.3.b – CLEO Compatibility with Zinc Bromide Brine 19.2 ppg (Lab Made) @ 20 °C

% v/v CLEO : % v/v ZnBr2

Brine 19.2ppg

Aging Time

Appearance before shaking Appearance after shaking



























99 : 1 3 weeks Two phases, both colourless clear and bright. Two phases, top clear and bright with brine bubbles,

bottom trace hazy.


bottom trace hazy.


bottom trace hazy.


bottom moderately hazy.


protocol.


protocol.


protocol.


protocol.


protocol.

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ISO 13628‐6 (2012)

89

CLEO Compatibility with Zinc Bromide Brine 19.2 ppg (Lab Made) @ 20 °C

Aging Time



99% CLEO :

1% ZnBr2 Brine

98% CLEO :

2% ZnBr2 Brine




99% CLEO :

1% ZnBr2 Brine

98% CLEO :

2% ZnBr2 Brine



1 day

1 week

2 week

3 week


protocol.

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ISO 13628‐6 (2012)

90

4.5.4.a – CLEO Compatibility with Cabot Potassium Formate Buffered 1.57 SG @ 5 °C

% v/v CLEO : % v/v K Formate 1.57 SG



























99.5 : 0.5 3 weeks Two phases, both colourless clear and bright. Bottom phase clear and bright, top phase trace hazy


99 : 1 3 weeks Two phases, both colourless clear and bright. Bottom phase clear and bright, top phase trace hazy




95 : 5 3 weeks Two phases, both colourless clear and bright. Bottom phase clear and bright, top phase slightly hazy


90 : 10 3 weeks Two phases, both colourless clear and bright. Bottom phase clear and bright, top phase slightly hazy

with some brine bubbles visible in oil phase


protocol.


protocol.


protocol.


protocol.


protocol.

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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

91

CLEO Compatibility with Cabot Potassium Formate Buffered 1.57 SG @ 5 °C

Aging

Time


99.5 %

CLEO :

0.5% K

Formate

Brine

99%

CLEO :

1% K

Formate

Brine

98%

CLEO :

2% K

Formate

Brine

95%

CLEO :

5% K

Formate

Brine

90%

CLEO :

10% K

Formate

Brine

99.5 %

CLEO :

0.5% K

Formate

Brine

99%

CLEO :

1% K

Formate

Brine

98%

CLEO :

2% K

Formate

Brine

95%

CLEO :

5% K

Formate

Brine

90%

CLEO :

10% K

Formate

Brine

1 day

1 week

2 week

3 week


protocol.

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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

92

4.5.4.b – CLEO Compatibility with Cabot Potassium Formate Buffered 1.57 SG @ 20 °C

% v/v CLEO : % v/v K Formate 1.57 SG

Aging Time


99.5 : 0.5 N/A Two phases, both colourless clear and

bright. Two clear & bright phases, brine bubbles in oil phase.

99 : 1 N/A Two phases, both colourless clear and








99.5 : 0.5 1 hour Two phases ‐ bottom clear and bright, top

trace hazy. Two phases, both trace hazy, brine bubbles in oil phase.

99 : 1 1 hour Two phases ‐ bottom clear and bright, top

trace hazy. Two phases, both trace hazy brine bubbles in oil phase.


trace hazy. Two phases, both slightly hazy brine bubbles in oil phase.


trace hazy. Two phases, both slightly hazy brine bubbles in oil phase.


trace hazy. Two phases, both moderately hazy brine bubbles in oil phase.

99.5 : 0.5 1 day Two phases ‐ both clear and bright. Two phases, both trace hazy, brine bubbles in oil phase.

99 : 1 1 day Two phases ‐ both clear and bright. Two phases, both trace hazy brine bubbles in oil phase.

98 : 2 1 day Two phases ‐ both clear and bright. Two phases, both slightly hazy brine bubbles in oil phase.

95 : 5 1 day Two phases ‐ both clear and bright. Two phases, both slightly hazy brine bubbles in oil phase.

90 : 10 1 day Two phases ‐ both clear and bright. Two phases, both moderately hazy brine bubbles in oil phase.

99.5 : 0.5 1 week Two phases ‐ both clear and bright. Two phases, both trace hazy, brine bubbles in oil phase.

99 : 1 1 week Two phases ‐ both clear and bright. Two phases, both trace hazy brine bubbles in oil phase.

98 : 2 1 week Two phases ‐ both clear and bright. Two phases, both slightly hazy brine bubbles in oil phase.

95 : 5 1 week Two phases ‐ both clear and bright. Two phases, both slightly hazy brine bubbles in oil phase.

90 : 10 1 week Two phases ‐ both clear and bright. Two phases, both moderately hazy brine bubbles in oil phase.

99.5 : 0.5 2 weeks Two phases ‐ both clear and bright. Two phases, both trace hazy, brine bubbles in oil phase.

99 : 1 2 weeks Two phases ‐ both clear and bright. Two phases, both trace hazy brine bubbles in oil phase.

98 : 2 2 weeks Two phases ‐ both clear and bright. Two phases, both slightly hazy brine bubbles in oil phase.


90 : 10 2 weeks Two phases ‐ both clear and bright. Two phases, both moderately hazy brine bubbles in oil phase.

99.5 : 0.5 3 weeks Two phases ‐ both clear and bright. Two phases, both trace hazy, brine bubbles in oil phase.

99 : 1 3 weeks Two phases ‐ both clear and bright. Two phases, both trace hazy brine bubbles in oil phase.



90 : 10 3 weeks Two phases ‐ both clear and bright. Two phases, both moderately hazy brine bubbles in oil phase.

99.5 : 0.5 4 weeks Two phases ‐ both clear and bright. Mixture not shaken after 4 weeks in line with testing protocol.

99 : 1 4 weeks Two phases ‐ both clear and bright. Mixture not shaken after 4 weeks in line with testing protocol.




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93

CLEO Compatibility with Cabot Potassium Formate Buffered 1.57 SG @ 20 °C

Aging

Time


99.5 %

CLEO :

0.5% K

Formate

Brine

99%

CLEO :

1% K

Formate

Brine

98%

CLEO :

2% K

Formate

Brine

95%

CLEO :

5% K

Formate

Brine

90%

CLEO :

10% K

Formate

Brine

99.5 %

CLEO :

0.5% K

Formate

Brine

99%

CLEO :

1% K

Formate

Brine

98%

CLEO :

2% K

Formate

Brine

95%

CLEO :

5% K

Formate

Brine

90%

CLEO :

10% K

Formate

Brine

1 day

1 week

2 week

3 week


protocol.

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TECHNICAL MANUAL TO

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94

4.5.5.a – CLEO Compatibility with Cabot Caesium Formate Buffered 2.20 SG @ 5 °C

% v/v CLEO : % v/v Cs Formate 2.20 SG








































protocol.


protocol.


protocol.


protocol.


protocol.

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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

95

CLEO Compatibility with Cabot Caesium Formate Buffered 2.20 SG @ 5 °C

Aging

Time


99.5 %

CLEO :

0.5% Cs

Formate

Brine

99%

CLEO :

1% Cs

Formate

Brine

98%

CLEO :

2% Cs

Formate

Brine

95%

CLEO :

5% Cs

Formate

Brine

90%

CLEO :

10% Cs

Formate

Brine

99.5 %

CLEO :

0.5% Cs

Formate

Brine

99%

CLEO :

1% Cs

Formate

Brine

98%

CLEO :

2% Cs

Formate

Brine

95%

CLEO :

5% Cs

Formate

Brine

90%

CLEO :

10% Cs

Formate

Brine

1 day

1 week

2 week

3 week


protocol.

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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

96

4.5.5.b – CLEO Compatibility with Cabot Caesium Formate Buffered 2.20 SG @ 20 °C

% v/v CLEO : % v/v Cs Formate 2.20 SG








































protocol.


protocol.


protocol.


protocol.


protocol.

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ISO 13628‐6 (2012)

97

CLEO Compatibility with Cabot Caesium Formate buffered 2.20 SG @ 20 °C

Aging

Time


99.5 %

CLEO :

0.5% Cs

Formate

Brine

99%

CLEO :

1% Cs

Formate

Brine

98%

CLEO :

2% Cs

Formate

Brine

95%

CLEO :

5% Cs

Formate

Brine

90%

CLEO :

10% Cs

Formate

Brine

99.5 %

CLEO :

0.5% Cs

Formate

Brine

99%

CLEO :

1% Cs

Formate

Brine

98%

CLEO :

2% Cs

Formate

Brine

95%

CLEO :

5% Cs

Formate

Brine

90%

CLEO :

10% Cs

Formate

Brine

1 day

1 week

2 week

3 week


protocol.

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98

4.6 – Compatibility with Miscellaneous Operational Fluids


The control fluid is mixed with other relevant operational fluids in the specified volume mixing

ratios at 5 °C (41 °F), and 20 °C (68 °F) and exposed for 4 wks.

PROCEDURE

The control fluid is mixed with the operational fluid in a mixing ratio which depends on the

secondary fluid. Mixing ratios are defined as control fluid : contaminant.

35% hydrochloric acid, in the following volume mixing ratios: 99.5:0.5; 99:1; 98:2; 95:5

and 90:10.

For methanol: 95:5; 90:10; 75:25 and 50:50.

Compensation fluids (HDEO): 95:5; 90:10; 75:25 and 50:50.

Silicon oil: 99:1

MEG: 100‐ and 1000 ppmw MEG in oil

The samples are exposed at 5°C (41°F) and 20°C (68°F) for 4 wk. The mixtures are shaken

vigorously on mixing and on intervals (1, 7, 14 and 21 days). The appearance of the mixtures and

formation of separations are observed instantly after being shaken, after 1 hour, 1 day, 1 week

and 4 weeks.

ACCEPTANCE CRITERIA

There are no general acceptance criteria related to this property. The results have to be evaluated

for the individual projects for which they are relevant. It is up to each specific project to define

project‐related criteria if this is considered necessary.

RESULTS

Results for each fluid mixture are outlined below for CLEO and results are broadly as expected

when mixing with miscellaneous operational fluids.

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99


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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

100

4.6.1.a – CLEO mixed with 35% HCl @ 5 °C from BDH ‐ Analar grade

%w/w of 35% HCl added

Aging Time


0.5 N/A Two phases colourless, clear and bright Single phase, slightly hazy and beginning to separate

0.5 1 hour Two phases colourless, clear and bright Single phase, slightly hazy and beginning to separate

0.5 1 day Two phases colourless, clear and bright Single phase, slightly hazy and beginning to separate

0.5 1 week Two Phases, colourless, clear and bright with

droplets on the bottom Single phase, slightly hazy and beginning to separate






droplets on the bottom Mixture not shaken after 4 weeks in line with testing

protocol.

1 N/A Two phases colourless, clear and bright Single phase, slightly hazy and beginning to separate

1 1 hour Two phases colourless, clear and bright Single phase, slightly hazy and beginning to separate

1 1 day Two phases colourless, clear and bright Single phase, slightly hazy and beginning to separate

1 1 week Two Phases, colourless, clear and bright with








protocol.




2 1 week Two phases, both colourless, clear and bright Single phase, slightly hazy and beginning to separate






protocol.










protocol.










protocol.

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101

CLEO mixed with 35% HCl @ 5 °C from BDH ‐ Analar grade

Aging Time


99.5 % CLEO :

0.5% HCl

99% CLEO : 1% HCl

98% CLEO : 2% HCl

95% CLEO : 5% HCl

90% CLEO : 10% HCl

99.5 % CLEO :

0.5% HCl

99% CLEO : 1% HCl

98% CLEO : 2% HCl

95% CLEO : 5% HCl

90% CLEO : 10% HCl

1 hour

1 day

1 week

2 week

3 week


protocol.

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102

4.6.1.b – CLEO mixed with 35% HCl @ 20 °C from BDH ‐ Analar grade

%w/w of 35% HCl added


0.5 N/A Two phases colourless, clear and bright Single phase, slightly hazy and beginning to separate

0.5 1 hour Two phases colourless, clear and bright Single phase, slightly hazy and beginning to separate

0.5 1 day Two phases colourless, clear and bright Single phase, slightly hazy and beginning to separate

0.5 1 week Two Phases, top, pale pink, clear and bright.

Bottom, colourless with clear droplets Single phase, pale pink, clear and bright with

aeration.


Bottom, colourless with clear droplets Single phase, pale pink, clear and bright.


Bottom, colourless with clear droplets Single phase, pale pink, clear and bright.


Bottom, colourless with clear droplets Mixture not shaken after 4 weeks in line with

testing protocol.




1 1 week Two Phases, top, pale pink, clear and bright.

Bottom, colourless with clear droplets Single phase, slightly hazy and beginning to separate







testing protocol.












testing protocol.












testing protocol.












testing protocol.

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103

CLEO mixed with 35% HCl @ 20 °C from BDH ‐ Analar grade

Aging Time


99.5 % CLEO :

0.5% HCl

99% CLEO : 1% HCl

98% CLEO : 2% HCl

95% CLEO : 5% HCl

90% CLEO : 10% HCl

99.5 % CLEO :

0.5% HCl

99% CLEO : 1% HCl

98% CLEO : 2% HCl

95% CLEO : 5% HCl

90% CLEO : 10% HCl

1 hour

1 day

1 week

2 week

3 week


protocol.

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104

4.6.2.a – CLEO mixed with methanol @ 5 °C from Sigma Aldrich ‐ ACS grade

%v/v of methanol added


5 N/A Two phases colourless, clear and bright Single phase, with light aeration

5 1 hour Single phase, colourless, clear and bright Single phase, with light aeration

5 1 day Single phase, colourless, clear and bright Single phase, with light aeration

5 1 week Single phase, colourless, clear and bright Single phase, with light aeration



5 4 week Single phase, colourless, clear and bright Mixture not shaken after 4 weeks in line with

testing protocol.








testing protocol.








testing protocol.



50 1 day Appears single phase, colourless, clear and bright,

but slight disturbance gave rise to 2 phases Single phase, with light aeration

50 1 week Two phases, both colourless, clear and bright Single phase, with light aeration



50 4 week Two phases, both colourless, clear and bright Mixture not shaken after 4 weeks in line with

testing protocol.

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105

CLEO mixed with methanol @ 5 °C from Sigma Aldrich ‐ ACS grade

Aging Time


95 % CLEO : 5% MeOH

90% CLEO : 10% MeOH

75% CLEO : 25% MeOH

50% CLEO : 50% MeOH

95 % CLEO : 5% MeOH

90% CLEO : 10% MeOH

75% CLEO : 25% MeOH

50% CLEO : 50% MeOH

1 hour

1 day

1 week

2 week

3 week


protocol.

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106

4.6.2.b – CLEO mixed with methanol @ 20 °C from Sigma Aldrich ‐ ACS grade

%v/v of methanol added




5 1 week Single phase, colourless, clear and bright Single phase, colourless, clear and bright



5 4 week Single phase, colourless, clear and bright Mixture not shaken after 4 weeks in line with testing

protocol.







protocol.







protocol.







protocol.

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ISO 13628‐6 (2012)

107

CLEO mixed with methanol @ 20 °C from Sigma Aldrich ‐ ACS grade

Aging Time


95 % CLEO : 5% MeOH

90% CLEO : 10% MeOH

75% CLEO : 25% MeOH

50% CLEO : 50% MeOH

95 % CLEO : 5% MeOH

90% CLEO : 10% MeOH

75% CLEO : 25% MeOH

50% CLEO : 50% MeOH

1 hour

1 day

1 week

2 week

3 week


protocol.

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108

4.6.3 – CLEO mixed with MEG from Niche Products Manufacturing Plant

ppmw of MEG added

Aging temperature

/ °C Aging Time Appearance before shaking Appearance after shaking

100 N/A N/A Single phase clear and bright Single phase clear and bright with light

aeration

100 5 1 hour Single phase clear and bright Single phase clear and bright with light

aeration

100 5 1 day Single phase clear and bright Single phase clear and bright with light

aeration

100 5 1 week Single phase clear and bright Single phase clear and bright with light

aeration


aeration


aeration

100 5 4 week Single phase clear and bright Mixture not shaken after 4 weeks in line with

testing protocol.


aeration


aeration


aeration


aeration


aeration


testing protocol.

1000 N/A N/A Droplets of MEG on bottom surface of

container Single phase clear and bright with light

aeration


aeration


aeration


aeration


aeration


aeration


testing protocol.


aeration


aeration


aeration


aeration


aeration


testing protocol.

Fluid Aging Temperature / °C Filterability ISO 13628‐6

CLEO + 100 ppm MEG 5 98.1% Pass

20 93.1% Pass

CLEO + 1000 ppm MEG 5 97.5% Pass

20 98.4% Pass

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109

CLEO mixed with MEG from Niche Products Manufacturing Plant aged @ 5°C

Aging Time


100 ppmw MEG 1000 ppmw MEG 100 ppmw MEG 1000 ppmw MEG

1 hour

1 day

1 week

2 week

3 week


protocol.

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110

CLEO mixed with MEG from Niche Products Manufacturing Plant aged @ 20°C

Aging Time


100 ppmw MEG 1000 ppmw MEG 100 ppmw MEG 1000 ppmw MEG

1 hour

1 day

1 week

2 week

3 week


protocol.

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ISO 13628‐6 (2012)

111


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112

4.6.4.a – CLEO mixed with HDEO @ 5 °C

%v/v of HDEO added



5 1 hour Single phase trace hazy Single phase, with light aeration

5 1 day Single phase trace hazy Single phase clear and bright with light aeration

5 1 week Single phase, colourless, trace hazy. Single phase, colourless, clear and bright

5 2 week Single phase, colourless, slightly hazy Single phase, colourless, clear and bright


5 4 week Single phase, colourless, slightly hazy Mixture not shaken after 4 weeks in line with testing

protocol.

10 N/A Two phases colourless, clear and bright Single phase, with moderate aeration

10 1 hour Single phase slightly hazy Single phase, with moderate aeration

10 1 day Single phase slightly hazy Single phase, slightly hazy with light aeration

10 1 week Single phase, colourless, hazy. Single phase, slightly hazy with aeration

10 2 week Single phase, colourless, hazy Single phase, colourless, slightly hazy

10 3 week Single phase, colourless, hazy Single phase, colourless, slightly hazy

10 4 week Single phase, colourless, hazy Mixture not shaken after 4 weeks in line with testing

protocol.


25 1 hour Single phase slightly hazy Single phase, with moderate aeration

25 1 day Single phase slightly hazy Single phase, slightly hazy with light aeration

25 1 week Single phase, colourless, hazy. Beginning to separate Single phase, slightly hazy with aeration




protocol.


50 1 hour Single phase clear and bright Single phase, with moderate aeration



50 1 week Single phase, colourless, slightly hazy Single phase, trace hazy with aeration

50 2 week Single phase, colourless, slightly hazy Single phase, colourless, trace hazy

50 3 week Single phase, colourless, slightly hazy Single phase, colourless, trace hazy


protocol.

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113

CLEO mixed with HDEO @ 5 °C

Aging Time


95 % CLEO : 5% HDEO

90% CLEO : 10% HDEO

75% CLEO : 25% HDEO

50% CLEO : 50% HDEO

95 % CLEO : 5% HDEO

90% CLEO : 10% HDEO

75% CLEO : 25% HDEO

50% CLEO : 50% HDEO

1 hour

1 day

1 week

2 week

3 week


protocol.

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114

4.6.4.b – CLEO mixed with HDEO @ 20 °C

%v/v of HDEO added



5 1 day Single phase, colourless, clear and bright Single phase clear and bright with light aeration





protocol.

10 1 hour Single phase clear and bright Single phase, with light aeration

10 1 day Single phase trace hazy Single phase trace hazy with moderate aeration

10 1 week Single phase, colourless, slightly hazy Single phase, colourless, slightly hazy with aeration

10 2 week Single phase, colourless, trace hazy Single phase, colourless, trace hazy

10 3 week Single phase, colourless, trace hazy Single phase, colourless, trace hazy

10 4 week Single phase, colourless, trace hazy Mixture not shaken after 4 weeks in line with testing

protocol.


25 1 day Single phase slightly hazy Single phase trace hazy with moderate aeration


25 2 week Single phase, colourless, slightly hazy Single phase, colourless, slightly hazy



protocol.


50 1 day Single phase slightly hazy Single phase trace hazy with moderate aeration





protocol.

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115

CLEO mixed with HDEO @ 20 °C

Aging Time


95 % CLEO : 5% HDEO

90% CLEO : 10% HDEO

75% CLEO : 25% HDEO

50% CLEO : 50% HDEO

95 % CLEO : 5% HDEO

90% CLEO : 10% HDEO

75% CLEO : 25% HDEO

50% CLEO : 50% HDEO

1 hour

1 day

1 week

2 week

3 week


protocol.

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116

4.6.5 – CLEO Compatibility with Silicone Oil (99:1 Ratio)

Temperature / °C Aging Time Appearance before shaking Appearance after shaking

5 1 hour Trace hazy fluid Moderately hazy fluid.

5 1 day Slightly hazy fluid Moderately hazy fluid.

5 1 week Slightly hazy fluid Moderately hazy fluid.



5 4 week Slightly hazy fluid Mixture not shaken after 4 weeks in line with testing protocol.

20 1 hour Two phases, clear and bright Two phases, clear and bright, aeration seen.

20 1 day Two phases, clear and bright Two phases, clear and bright, aeration seen.

20 1 week Two phases, clear and bright Two phases, clear and bright, aeration seen.



20 4 week Two phases, clear and bright Mixture not shaken after 4 weeks in line with testing protocol.

Aging Temp.

1 hour 1 day 1 week 2 week 3 week 4 week

5 °C Before Mixing

5 °C After Mixing


Aging Temp.

1 hour 1 day 1 week 2 week 3 week 4 week

20 °C Before Mixing

20 °C After Mixing


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117

4.7 – Metal Compatibility

4.7.1 – Metal Compatibilities at 70 °C


Tests are carried out in the neat fluid and aged for 3 weeks, 6 weeks and 12 weeks following the

methodology laid out in ISO 16328‐6 Annex C Protocol with the following deviations / extensions.

The test pieces were aged at 70 °C, which is more severe than the 60 °C testing required

in ISO 13628‐6

The following methods are used to evaluate compatibility:

change in appearance of fluid relative to unused fluid;

appearance and amount of solid deposits (particles, sludge) in the fluid and on the metal

samples;

qualitative description of corrosion products and corrosion attacks (attacks which are

clearly related to edges or fixture holes are disregarded);

mass loss as a function of time, transformed into micrometres per year uniform corrosion;

PROCEDURE

The ready‐made metal samples, which have a standard surface area and a standard surface

condition, are degreased, dried and weighed to the nearest 0.1 mg and then immersed in both

the neat control fluid, and in the presence of 10% sea water. It should be noted that when sea

water is present, the metal is exposed completely in the control fluid phase and not the sea water

phase.

Tests were carried out in glass vessels at 70 °C. Each of the individual metals is exposed in a

separate container in a number of nine replicate specimens, with three replicates are retrieved

from the fluid after 3 weeks, 6 weeks and 12 weeks. After visual inspection of the samples and

after appropriate cleaning, weight loss is measured and the samples inspected for visible

corrosion attacks, which are characterized. The weight losses are transcribed into uniform

corrosion, in micrometres per year, and maximum depth of local attacks, in micrometres, is

determined under a microscope with a calibrated depth of focus. The fluid is inspected for any

separations, including solid particles or sludge.

ACCEPTANCE CRITERIA

No substantial visible corrosion products or attacks on any of the metals,

No significant amounts of deposits (particles or sludge) in the fluid at the end of the test

period,

Corrosion rates shall show a clear declining tendency with time.

Corrosion rate of the carbon steel including galvanic coupling shall not exceed 10 μm/year

(12 weeks result).

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118

Corrosion rate of AISI 316 shall not exceed 5 μm/year (12 weeks result). Maximum depth

of local attacks shall not exceed 25 μm.

Corrosion rate of 17‐4PH shall not exceed 5 μm/year (12 weeks result) and maximum

depth of local attacks shall not exceed 25 μm.

Corrosion rate of electroless nickel shall not exceed 2 µm/year (12 weeks result)

RESULTS

Tests complete for all materials. All results for 3, 6, and 12 weeks shown below indicate that all

the test pieces passed the ISO 13628‐6 specification. No issues were observed for CLEO after 12

weeks with all metals tested.

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119

SUMMARY OF METAL RESULTS FOR CLEO AT 70 °C

The following metals have completed 12 weeks aging @ 70 °C in accordance with ISO 13628‐6.

Metal CLEO No Sea Water CLEO with 10% Sea Water

ISO 13628‐6 Comments ISO 13628‐6 Comments

17 – 4 – PH UNS S17400 Pass Pass

316Ti Pass Pass

A182 F51 UNS S31803 / A890 GR4A (Super

Duplex) Pass Pass

A182 F53 UNS 32750 (Super Duplex) Pass Pass

AISI A29 4340 Gas Nitrided Pass Pass

AISI A29 4340 Pass Pass

AISI A350 LF2 Carbon Steel Pass Pass

AISI 410 Pass Pass

AISI 420 Pass Pass

AISI 430 Pass Pass

AISI 4140 Pass Pass

AISI 440C Pass Pass

AISI 1040 Pass Pass

AISI 6150 Pass Pass

AlCNC10 Pass Pass

Alloy 3 Pass Slight darkening of metal Pass Darkening of metal

Aluminium Bronze HM9843 Pass Pass Dulling of metal

Aluminium Bronze UNS C63000 Pass Slight darkening of metal Pass Dulling of metal

ASTM B418 Aluminium Bronze Pass Pass Slight darkening of metal

Becol UNS C17200 Pass Pass Slight darkening of metal

Carbon Steel UNS K02401 Pass Pass

Chrome Core Pass Pass

Copper Pass Pass Slight darkening of metal

CuAl10Ni Pass Minor darkening Pass Minor staining

DGS1043 Pass Pass Moderate staining

Duplex 9490 Pass Pass

Elgiloy Pass Pass

Electroless Nickel Plated Steel Pass Pass

Everslik 1201 Coating Pass Pass

Everslik 1201/1301 Coating Pass Pass

Inconel 625 Pass Pass


Inconel 718 Ag Coated Pass Pass Minor colouration

Inconel 718 Gold Coated Pass Pass

Inconel 725 GV50H Pass Pass

Inconel 725 Ag Coated Pass Pass Minor colouration



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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

120

Metal CLEO No Sea Water CLEO with 10% Sea Water

ISO 13628‐6 Comments ISO 13628‐6 Comments

KR16 Pass Pass

Mild Steel Pass Trace darkening Pass

Monel Alloy 400 Pass Pass

Monel Alloy K500 Pass Pass

MP35N Pass Pass

Nitronic 50 Pass Pass

Phosphor Bronze PB102 Pass Pass Dulling of metal

Super Duplex Cameron Pass Pass

Super Duplex AM8831 Pass Pass

Super Duplex UNS S32760 Pass Pass

Silicon Nitride Pass Pass

Stainless Steel 304 Pass Pass




Titanium Pass Pass

Toughmet 3 (UNS C72900)

Annealing condition 308 AJU Pass Pass


Annealing condition 308 ANB Pass Pass


Annealing condition 309 AAE Pass Pass

TP19D Pass Pass

Zirconia Pass Pass

Zinc Plated Washer Pass Pass

10% Ni Bonded Tungsten Carbide Pass Pass

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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

121

4.7.1.1.a ‐ CLEO (Neat) ‐ Multiple Piece Corrosion Testing (3 week data)

Metal Appearance of metal Appearance of fluid

(solids / sludge)

Initial

Weight /

g

Aged

Weight /

g

weight

loss / mg

Corrosion

rate (µm

per annum)

Stainless

Steel 316

Clear and

bright

Fluid clear and

bright, no solids

seen

55.0805 55.0807 ‐0.2 ‐0.14

55.0887 55.089 ‐0.3 ‐0.21

55.7968 55.7968 0 0.00

17‐4‐PH

UNS

S17400

Clear and

bright

Fluid clear and

bright, no solids

seen

99.4731 99.4743 ‐1.2 ‐0.88

99.5038 99.5054 ‐1.6 ‐1.17

99.5948 99.5962 ‐1.4 ‐1.02

Beryllium

Copper

UNS

C17200

Slight

discolouration

of metal

Fluid clear and

bright, no solids

seen

106.1152 106.1155 ‐0.3 ‐0.21

107.169 107.1693 ‐0.3 ‐0.21

106.2265 106.227 ‐0.5 ‐0.35

Aluminium

Bronze UNS

C63000

Slight

discolouration

of metal

Fluid clear and

bright, no solids

seen

96.7134 96.7148 ‐1.4 ‐1.04

96.2969 96.2984 ‐1.5 ‐1.12

96.952 96.9536 ‐1.6 ‐1.19

10% Nickel

Bonded

Tungsten

Carbide

Clear and

bright

Fluid clear and

bright no solids

seen.

11.0026 11.0028 ‐0.2 ‐0.41

11.0506 11.0504 0.2 0.41

11.0792 11.0793 ‐0.1 ‐0.21

Electroless

Plated

Nickel

Clear and

bright

Fluid clear and

bright no solids

seen.

6.9102 6.9101 0.1 0.09

6.6669 6.6668 0.1 0.09

7.2024 7.2022 0.2 0.17

Carbon

Steel UNS

K02401

Clear and

bright

Fluid clear and

bright no solids

seen.

18.0974 18.0978 ‐0.4 ‐0.31

16.6828 16.6829 ‐0.1 ‐0.08

17.9585 17.9585 0 0.00

All metals pass the ISO 13628‐6 specification indicating excellent compatibility with CLEO.

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TECHNICAL MANUAL TO

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122

4.7.1.1.b ‐ CLEO (Neat) ‐ Multiple Piece Corrosion Testing (6 week data)


(solids / sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Stainless

Steel 316 Clear and bright

Fluid clear and

bright, no solids

seen

55.0805 55.0809 ‐0.4 ‐0.14

55.0887 55.0896 ‐0.9 ‐0.32

55.7968 55.797 ‐0.2 ‐0.07

17‐4‐PH

UNS

S17400

Clear and bright

Fluid clear and

bright, no solids

seen

99.4731 99.4737 ‐0.6 ‐0.22

99.5038 99.5047 ‐0.9 ‐0.33

99.5948 99.5957 ‐0.9 ‐0.33

Beryllium

Copper

UNS

C17200

Slight discolouration

of metal.

Fluid clear and

bright, no solids

seen

106.1152 106.1142 1 0.35

107.169 107.1679 1.1 0.38

106.2265 106.2256 0.9 0.31

Aluminium

Bronze UNS

C63000


of metal.

Fluid clear and

bright, no solids

seen

96.7134 96.7136 ‐0.2 ‐0.07

96.2969 96.2971 ‐0.2 ‐0.07

96.952 96.9524 ‐0.4 ‐0.15

10% Nickel

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright no solids

seen.

11.0026 11.0028 ‐0.2 ‐0.21

11.0506 11.0505 0.1 0.10

11.0792 11.0793 ‐0.1 ‐0.10

Electroless

Plated

Nickel

Clear and bright

Fluid clear and

bright no solids

seen.

6.9102 6.9103 ‐0.1 ‐0.04

6.6669 6.667 ‐0.1 ‐0.04

7.2024 7.2025 ‐0.1 ‐0.04

Carbon

Steel UNS

K02401

Clear and bright

Fluid clear and

bright no solids

seen.

18.0974 18.0975 ‐0.1 ‐0.04

16.6828 16.6829 ‐0.1 ‐0.04

17.9585 17.9585 0 0.00


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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

123

4.7.1.1.c ‐ CLEO (Neat) ‐ Multiple Piece Corrosion Testing (12 week data)


(solids / sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Stainless


Fluid clear and

bright, no solids

seen

55.0805 55.0812 ‐0.7 ‐0.12

55.0887 55.0895 ‐0.8 ‐0.14

55.7968 55.797 ‐0.2 ‐0.04

17‐4‐PH

(UNS

S17400)

Clear and bright

Fluid clear and

bright, no solids

seen

99.4731 99.4749 ‐1.8 ‐0.33

99.5038 99.5058 ‐2 ‐0.37

99.5948 99.5966 ‐1.8 ‐0.33

Beryllium

Copper

UNS

C17200


of metal

Fluid clear and

bright, no solids

seen

106.1152 106.116 ‐0.8 ‐0.14

107.1690 107.1697 ‐0.7 ‐0.12

106.2265 106.2276 ‐1.1 ‐0.19

Aluminium

Bronze UNS

C63000


of metal

Fluid clear and

bright, no solids

seen

96.7134 96.7152 ‐1.8 ‐0.34

96.2969 96.2988 ‐1.9 ‐0.35

96.952 96.954 ‐2 ‐0.37

10% Nickel

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright no solids

seen.

11.0026 11.0028 ‐0.2 ‐0.21

11.0506 11.0505 0.1 0.10

11.0792 11.0793 ‐0.1 ‐0.10

Electroless

Plated

Nickel

Clear and bright

Fluid clear and

bright no solids

seen.

6.9102 6.9101 0.1 0.02

6.6669 6.6667 0.2 0.04

7.2024 7.2022 0.2 0.04

Carbon

Steel UNS

K02401

Clear and bright

Fluid clear and

bright, no solids

seen

18.0974 18.0978 ‐0.4 ‐0.08

16.6828 16.683 ‐0.2 ‐0.04

17.9585 17.9585 0 0.00


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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

124

4.7.1.2.a ‐ CLEO with 10% Sea Water ‐ Multiple Piece Corrosion Testing (3 week data)


(solids / sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Stainless

Steel 316

Clear and

bright

Fluid clear and

bright*.

No Solids Seen.

56.1237 56.1246 ‐0.9 ‐0.64

55.3632 55.3644 ‐1.2 ‐0.85

54.9706 54.9725 ‐1.9 ‐1.35

17‐4‐PH

(UNS

S17400)

Clear and

bright

Fluid clear and

bright*.

No Solids Seen.

99.4931 99.4941 ‐1 ‐0.73

99.7512 99.7521 ‐0.9 ‐0.66

99.5319 99.533 ‐1.1 ‐0.80

Beryllium

Copper

UNS

C17200

Slight

darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

105.3943 105.396 ‐1.7 ‐1.18

105.2525 105.2541 ‐1.6 ‐1.11

106.4434 106.4451 ‐1.7 ‐1.18

Aluminium

Bronze UNS

C63000

Clear and

bright

Fluid clear and

bright*.

No Solids Seen.

95.4597 95.461 ‐1.3 ‐0.97

96.4847 96.4858 ‐1.1 ‐0.82

96.2957 96.2971 ‐1.4 ‐1.05

10% Nickel

Bonded

Tungsten

Carbide

Clear and

bright

Fluid clear and

bright*.

No Solids Seen.

11.0431 11.0427 0.4 0.83

11.0348 11.0346 0.2 0.41

11.0383 11.0383 0 0.00

Electroless

Plated

Nickel

Clear and

bright

Fluid clear and

bright*.

No Solids Seen.

6.8225 6.823 ‐0.5 ‐0.43

6.7457 6.746 ‐0.3 ‐0.26

6.7903 6.7907 ‐0.4 ‐0.34

Carbon

Steel UNS

K02401

Clear and

bright

Fluid clear and

bright*.

No Solids Seen.

18.0428 18.0431 ‐0.3 ‐0.23

18.0411 18.0411 0 0.00

18.0978 18.0979 ‐0.1 ‐0.08


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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

125

4.7.1.2.b ‐ CLEO with 10% Sea Water ‐ Multiple Piece Corrosion Testing (6 week data)


(solids / sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Stainless


Fluid clear and

bright*.

No Solids Seen.

56.1237 56.1239 ‐0.2 ‐0.07

55.3632 55.3645 ‐1.3 ‐0.46

54.9706 54.9717 ‐1.1 ‐0.39

17‐4‐PH

(UNS

S17400)

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

99.4931 99.4924 0.7 0.25

99.7512 99.7504 0.8 0.29

99.5319 99.5317 0.2 0.07

Beryllium

Copper

UNS

C17200

Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

105.3943 105.3953 ‐1 ‐0.35

105.2525 105.2532 ‐0.7 ‐0.24

106.4434 106.444 ‐0.6 ‐0.21

Aluminium

Bronze UNS

C63000

Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

95.4597 95.4598 ‐0.1 ‐0.04

96.4847 96.4848 ‐0.1 ‐0.04

96.2957 96.296 ‐0.3 ‐0.11

10% Nickel

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

11.0431 11.0429 0.2 0.21

11.0348 11.0345 0.3 0.31

11.0383 11.0382 0.1 0.10

Electroless

Plated

Nickel

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

6.8225 6.8227 ‐0.2 ‐0.09

6.7457 6.7447 1 0.43

6.7903 6.7902 0.1 0.04

Carbon

Steel UNS

K02401

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

18.0428 18.0429 ‐0.1 ‐0.04

18.0411 18.0411 0 0.00

18.0978 18.0977 0.1 0.04


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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

126

4.7.1.2.c ‐ CLEO with 10% Sea Water ‐ Multiple Piece Corrosion Testing (12 week data)


(solids / sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Stainless


Fluid clear and

bright*.

No Solids Seen.

56.1237 56.1249 ‐1.2 ‐0.21

55.3632 55.3645 ‐1.3 ‐0.23

54.9706 54.9727 ‐2.1 ‐0.37

17‐4‐PH

(UNS

S17400)

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

99.4931 99.4947 ‐1.6 ‐0.29

99.7512 99.7525 ‐1.3 ‐0.24

99.5319 99.5333 ‐1.4 ‐0.25

Beryllium

Copper

UNS

C17200

Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

105.3943 105.3947 ‐0.4 ‐0.07

105.2525 105.2506 1.9 0.33

106.4434 106.4423 1.1 0.19

Aluminium

Bronze UNS

C63000

Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

95.4597 95.4609 ‐1.2 ‐0.22

96.4847 96.486 ‐1.3 ‐0.24

96.2957 96.297 ‐1.3 ‐0.24

10% Nickel

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

11.0431 11.0429 0.2 0.10

11.0348 11.0344 0.4 0.21

11.0383 11.0382 0.1 0.05

Electroless

Plated

Nickel

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

6.8225 6.8222 0.3 0.06

6.7457 6.7444 1.3 0.28

6.7903 6.79 0.3 0.06

Carbon

Steel UNS

K02401

Clear and bright, light

markings were

spacers contacted.

Fluid clear and

bright*.

No Solids Seen.

18.1016 18.102 ‐0.4 ‐0.08

17.9866 17.987 ‐0.4 ‐0.08

16.6262 16.6262 0 0.00


4.7.2 – Further Metal Compatibilities at 70 °C

The compatibility of a wider range of metals with CLEO has been undertaken based on the ISO

16328‐6 Annex C Protocol with the following deviations / extensions both for the neat fluid and

in the presence of 10% sea water:‐

Single or multiple piece testing was undertaken at 70 °C only.

The same test pieces were re‐immersed in the test fluid in order to obtain the results

after 3, 6 and 12 weeks.

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TECHNICAL MANUAL TO

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127

4.7.2.1.a ‐ CLEO (Neat) Metals Compatibility at 70 °C (3 week data)

Metal Appearance of metal

Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

17 – 4 – PH

UNS

S17400

Clear and bright

Fluid clear and

bright, no solids

seen

99.4731 99.4743 ‐1.2 ‐0.88

316 Ti Clear and bright

Fluid clear and

bright, no solids

seen

9.2972 9.2974 ‐0.20 ‐0.48

A182 F51

UNS

S31803 /

A890 GR4A

(Super

Duplex)

Clear and bright

Fluid clear and

bright, no solids

seen

97.2553 97.2568 ‐1.50 ‐1.11

A182 F53

UNS 32750

(Super

Duplex)

Clear and bright

Fluid clear and

bright, no solids

seen

61.1956 61.1963 0.1 0.10

AlCNC10 Clear and bright

Fluid clear and

bright, no solids

seen

2.3364 2.3364 0.50 0.42

AISI A29

4340 Gas

Nitrided

Clear and bright

Fluid clear and

bright, no solids

seen

94.9842 94.9859 ‐1.70 ‐1.20

AISI A29

4340 Clear and bright

Fluid clear and

bright, no solids

seen

88.2251 88.2251 0 0.00

AISI A350

LF2 Carbon

Steel

Clear and bright

Fluid clear and

bright, no solids

seen

95.6857 95.6878 ‐2.10 ‐1.49

AISI 410 Clear and bright

Fluid clear and

bright, no solids

seen

123.3737 123.3745 ‐0.80 ‐0.47


Fluid clear and

bright, no solids

seen

123.7503 123.7511 ‐0.80 ‐0.46


Fluid clear and

bright, no solids

seen

160.0036 160.0038 ‐0.20 ‐0.10


Fluid clear and

bright, no solids

seen

161.9419 161.9392 2.7 1.38

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128


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright, no solids

seen

308.42 308.44 ‐20 ‐6.85


Fluid clear and

bright, no solids

seen

96.4047 96.4041 0.60 0.45


Fluid clear and

bright, no solids

seen

156.2514 156.2494 2 1.05

Aluminium

Bronze

HM9843

Clear and bright

Fluid clear and

bright, no solids

seen

97.7409 97.7428 ‐0.4 ‐0.33

Aluminium

Bronze UNS

C63000

Clear and bright

Fluid clear and

bright, no solids

seen

96.7134 96.7148 ‐1.4 ‐1.04

Alloy 3 Clear and bright

Fluid clear and

bright, no solids

seen

10.4013 10.4013 0.00 0.00

ASTM B418

Aluminium

Bronze

Clear and bright

Fluid clear and

bright, no solids

seen

87.8577 87.8585 ‐0.8 ‐1.02

Becol

UNS

C17200

Slight darkening of

metal.

Fluid clear and

bright, no solids

seen

106.1152 106.1155 ‐0.3 ‐0.21

Carbon

Steel UNS

K02401

Clear and bright

Fluid clear and

bright, no solids

seen

18.0598 18.0602 ‐0.4 ‐0.31

Chrome

Core Clear and bright

Fluid clear and

bright, no solids

seen

3.7174 3.7176 ‐0.20 ‐1.26

Copper Clear and bright

Fluid clear and

bright, no solids

seen

49.8892 49.8893 ‐0.1 ‐0.04

CuAl10Ni Clear and bright

Fluid clear and

bright, no solids

seen

8.8022 8.8024 ‐0.20 ‐0.45

DGS1043 Clear and bright

Fluid clear and

bright, no solids

seen

4.968 4.9679 0.10 0.22

Duplex


Fluid clear and

bright, no solids

seen

156.5329 156.5331 ‐0.20 ‐0.10

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129


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Electro

Nickel

Plated

Clear and bright

Fluid clear and

bright, no solids

seen

6.9102 6.9101 0.1

Elgiloy Clear and bright

Fluid clear and

bright, no solids

seen

0.9924 0.9925 ‐0.10 ‐1.27

Inconel 625 Clear and bright

Fluid clear and

bright, no solids

seen

174.7289 174.7316 1.30 0.59


Fluid clear and

bright, no solids

seen

9.6885 9.6887 ‐0.20 ‐0.47

Inconel 718

Ag Coated Clear and bright

Fluid clear and

bright, no solids

seen

8.7772 8.7773 ‐0.10 ‐0.26

Inconel 718

Gold Plated Clear and bright

Fluid clear and

bright, no solids

seen

0.5792 0.5792 0 0.00

Inconel 725

GV50H Clear and bright

Fluid clear and

bright, no solids

seen

10.3738 10.3739 ‐0.10 ‐0.07


Fluid clear and

bright, no solids

seen

170.3522 170.3555 ‐3.3 ‐1.61

Inconel 725


Fluid clear and

bright, no solids

seen

37.6248 37.6256 ‐0.80 ‐1.86


Fluid clear and

bright, no solids

seen

158.7374 158.7374 0 0.00

KR16 Clear and bright

Fluid clear and

bright, no solids

seen

17.8924 17.8927 ‐0.30 ‐0.37

Mild Steel Clear and bright

Fluid clear and

bright, no solids

seen

45.2389 45.2395 ‐0.6 ‐0.30

Monel Alloy


Fluid clear and

bright, no solids

seen

149.3270 149.3270 0.00 0.00

Monel Alloy

K500 Clear and bright

Fluid clear and

bright, no solids

seen

174.102 174.1014 0.60 0.27

MP35N Clear and bright

Fluid clear and

bright, no solids

seen

10.0089 10.0090 ‐0.10 ‐0.23

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130


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Nitronic 50 Clear and bright

Fluid clear and

bright, no solids

seen

0.772 0.7720 0.00 0.00

Phosphor

Bronze

PB102

Clear and bright

Fluid clear and

bright, no solids

seen

177.397 177.4009 ‐3.9 ‐1.83

Super

Duplex

AM8831

Clear and bright

Fluid clear and

bright, no solids

seen

156.4496 156.4531 ‐3.5 ‐1.78

Super

Duplex UNS

S32760

Clear and bright

Fluid clear and

bright, no solids

seen

107.7365 107.74 ‐0.50 ‐0.35

Silicon

Nitride Clear and bright

Fluid clear and

bright, no solids

seen

3.502 3.5021 ‐0.10 ‐1.04

Stainless


Fluid clear and

bright, no solids

seen

44.4013 44.4022 ‐0.9 ‐0.45

Stainless


Fluid clear and

bright, no solids

seen

55.7968 55.7968 0 0.00

Stainless


Fluid clear and

bright, no solids

seen

151.314 151.3157 ‐1.70 ‐0.91

Stainless


Fluid clear and

bright, no solids

seen

154.1852 154.188 ‐2.80 ‐1.49

Super

Duplex

Cameron

Clear and bright

Fluid clear and

bright, no solids

seen

9.1622 9.1625 ‐0.30 ‐0.74

Titanium Clear and bright

Fluid clear and

bright, no solids

seen

87.7966 87.7991 ‐2.5 ‐2.35

Toughmet 3

AT110 (UNS

C72900)

Copper

Nickel Tin

Alloy, AMS

4596, ASTM

B 929

Annealing Condition

AJU

Clear and bright

Fluid clear and

bright, no solids

seen

31.7061 31.7067 ‐0.6 ‐0.62

Annealing Condition

ANB

Clear and bright

Fluid clear and

bright, no solids

seen

31.7143 31.7138 0.5 0.51

Annealing Condition

AAE

Clear and bright

Fluid clear and

bright, no solids

seen

31.657 31.6577 ‐0.7 ‐0.72

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131


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Umbilical

TP19D Clear and bright

Fluid clear and

bright, no solids

seen

15.7842 15.7842 0.00 0.00

Zirconia Clear and bright

Fluid clear and

bright, no solids

seen

6.524 6.5240 0.00 0.00

Zn plated

Washer Clear and bright

Fluid clear and

bright, no solids

seen

5.2813 5.2812 0.10 0.25

6% Ni

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright, no solids

seen

11.2051 11.2051 0.00 0.00

10% Ni

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright, no solids

seen

11.0026 11.0028 ‐0.20 ‐0.41

Coating Type Appearance of coating

Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Electro

Nickel

Plated‐PTFE

Opticote 450

Clear and bright

Fluid clear and

bright, no solids

seen

150.6769 150.6755 1.4 0.69

Everslik 1301 Clear and bright

Fluid clear and

bright, no solids

seen

44.4342 44.4352 ‐1.0 ‐0.49

Everslik

1201/1301 Clear and bright

Fluid clear and

bright, no solids

seen

44.5610 44.5619 ‐0.9 ‐0.44

Xylan 1014 Clear and bright

Fluid clear and

bright, no solids

seen

1.2416 1.2407 0.9 2.86


Fluid clear and

bright, no solids

seen

1.3881 1.3889 ‐0.8 ‐2.09


Fluid clear and

bright, no solids

seen

2.3055 2.3061 ‐0.6 ‐1.27


Fluid clear and

bright, no solids

seen

2.4051 2.405 0.1 0.00


Fluid clear and

bright, no solids

seen

1.567 1.5671 ‐0.1 ‐0.78


Fluid clear and

bright, no solids

seen

3.4908 3.4923 ‐1.5 ‐1.67

All metals conform to the ISO 13628‐6 specification showing excellent compatibility with CLEO.

Yellow metal test pieces show slight discolouration suggesting slight oxidation of the surface.

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ISO 13628‐6 (2012)

132

4.7.2.1.b ‐ CLEO (Neat) Metals Compatibility at 70 °C (6 week data)


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

17 – 4 – PH

UNS

S17400

Clear and bright

Fluid clear and

bright, no solids

seen

99.4731 99.4737 ‐0.6 ‐0.22

316Ti Clear and bright

Fluid clear and

bright, no solids

seen

9.2972 9.2975 ‐0.40 ‐0.48

A182 F51

UNS

S31803 /

A890 GR4A

(Super

Duplex)

Clear and bright

Fluid clear and

bright, no solids

seen

97.2553 97.2551 0.20 0.07

A182 F53

UNS 32750

(Super

Duplex)

Clear and bright

Fluid clear and

bright, no solids

seen

61.1956 61.1958 0.6 0.30


Fluid clear and

bright, no solids

seen

2.3364 2.3364 0.00 ‐0.07

AISI A29

4340 Gas

Nitrided

Clear and bright

Fluid clear and

bright, no solids

seen

94.9842 94.9845 ‐0.30 ‐0.11

AISI A29


Fluid clear and

bright, no solids

seen

88.2251 88.2249 0.2 0.07

AISI A350

LF2 Carbon

Steel

Clear and bright

Fluid clear and

bright, no solids

seen

95.6857 95.6861 ‐0.40 ‐0.14


Fluid clear and

bright, no solids

seen

123.3737 123.3745 ‐0.8 ‐0.24


Fluid clear and

bright, no solids

seen

123.7503 123.7509 ‐0.6 ‐0.17


Fluid clear and

bright, no solids

seen

160.0036 160.0035 0.1 0.03


Fluid clear and

bright, no solids

seen

161.9419 161.9391 2.8 0.72

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133


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright, no solids

seen

308.42 308.46 ‐40 ‐6.85


Fluid clear and

bright, no solids

seen

96.4047 96.4061 ‐1.40 ‐0.52


Fluid clear and

bright, no solids

seen

156.2514 156.2493 2.1 0.55

Aluminium

Bronze

HM9843

Clear and bright

Fluid clear and

bright, no solids

seen

97.7409 97.7412 1.2 0.49

Aluminium

Bronze UNS

C63000

Clear and bright

Fluid clear and

bright, no solids

seen

96.7134 96.7136 ‐0.2 ‐0.07


Fluid clear and

bright, no solids

seen

10.4013 10.4013 0.00 0.00

ASTM B418

Aluminium

Bronze

Clear and bright

Fluid clear and

bright, no solids

seen

87.8577 87.8606 ‐2.1 ‐1.33

Becol

UNS

C17200

Slight darkening of

metal.

Fluid clear and

bright, no solids

seen

106.1152 106.1142 1 0.35

Carbon

Steel UNS

K02401

Clear and bright

Fluid clear and

bright, no solids

seen

18.0598 18.0599 ‐0.1 ‐0.04

Chrome


Fluid clear and

bright, no solids

seen

3.7174 3.7177 ‐0.30 ‐0.95


Fluid clear and

bright, no solids

seen

49.8892 49.8892 0.1 0.02


Fluid clear and

bright, no solids

seen

8.8022 8.8023 ‐0.10 ‐0.11

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134


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright, no solids

seen

4.968 4.9678 0.20 0.22

Duplex


Fluid clear and

bright, no solids

seen

156.5329 156.5338 ‐0.90 ‐0.23

Electro

Nickel

Plated

Clear and bright

Fluid clear and

bright, no solids

seen

6.9102 6.9103 ‐0.1


Fluid clear and

bright, no solids

seen

0.9924 0.9924 0.00 0.00


Fluid clear and

bright, no solids

seen

174.7289 174.7276 1.3 0.3


Fluid clear and

bright, no solids

seen

9.6885 9.6887 ‐0.20 ‐0.23

Inconel 718


Fluid clear and

bright, no solids

seen

8.7772 8.7775 ‐0.20 ‐0.26

Inconel 718

Gold

Coated

Clear and bright

Fluid clear and

bright, no solids

seen

0.5616 0.5616 0.00 0.00

Inconel 725


Fluid clear and

bright, no solids

seen

10.3738 10.3739 0.00 0.00

Inconel 725


Fluid clear and

bright, no solids

seen

37.6248 37.6254 ‐0.60 ‐0.70


Fluid clear and

bright, no solids

seen

170.3522 170.3538 ‐1.6 ‐0.39


Fluid clear and

bright, no solids

seen

158.7374 158.7377 ‐0.3 ‐0.08

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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

135


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright, no solids

seen

17.8924 17.8910 1.40 0.86

Mild Steel Clear and bright

Fluid clear and

bright, no solids

seen

45.2389 45.2391 ‐0.2 ‐0.05

Monel Alloy


Fluid clear and

bright, no solids

seen

149.3270 149.3276 ‐0.6 ‐0.15

Monel Alloy


Fluid clear and

bright, no solids

seen

174.1020 174.1015 0.5 0.11


Fluid clear and

bright, no solids

seen

10.0089 10.0089 0.00 0.00


Fluid clear and

bright, no solids

seen

0.772 0.7719 0.10 0.38

Phosphor

Bronze

PB102

Very slight stain

Fluid clear and

bright, no solids

seen

177.397 177.3981 ‐1.1 ‐0.26

Super

Duplex

AM8831

Clear and bright

Fluid clear and

bright, no solids

seen

156.4496 156.4506 ‐1 ‐0.25

Super

Duplex UNS

S32760

Clear and bright

Fluid clear and

bright, no solids

seen

107.7365 107.74 ‐0.20 ‐0.07

Silicon


Fluid clear and

bright, no solids

seen

3.5020 3.5021 ‐0.1 ‐0.52

Stainless


Fluid clear and

bright, no solids

seen

44.4013 44.4015 ‐0.2 ‐0.05

Stainless


Fluid clear and

bright, no solids

seen

55.7968 55.797 ‐0.2 ‐0.07

Stainless


Fluid clear and

bright, no solids

seen

151.314 151.3136 0.40 0.11

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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

136


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Stainless


Fluid clear and

bright, no solids

seen

154.1852 154.1858 ‐0.60 ‐0.16

Super

Duplex

Cameron

Clear and bright

Fluid clear and

bright, no solids

seen

9.1622 9.1624 ‐0.20 ‐0.25


Fluid clear and

bright, no solids

seen

87.7966 87.7974 ‐0.8 ‐0.38

Toughmet 3

AT110 (UNS

C72900)

Copper

Nickel Tin

Alloy, AMS

4596, ASTM

B 929

Annealing Condition

AJU

Clear and bright

Fluid clear and

bright, no solids

seen

31.7061 31.7068 ‐0.7 ‐0.36

Annealing Condition

ANB

Clear and bright

Fluid clear and

bright, no solids

seen

31.7143 31.7147 ‐0.4 ‐0.21

Annealing Condition

AAE

Clear and bright

Fluid clear and

bright, no solids

seen

31.657 31.6575 0.3 0.15


Fluid clear and

bright, no solids

seen

15.7842 15.7842 0.00 0.00


Fluid clear and

bright, no solids

seen

6.5240 6.5240 0.00 0.00

Zn plated


Fluid clear and

bright, no solids

seen

5.2813 5.2812 0.10 0.12

6% Ni

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright, no solids

seen

11.2051 11.2051 0.00 0.00

10% Ni

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright, no solids

seen

11.0026 11.0028 ‐0.2 ‐0.21

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137

Coating Type Appearance of coating

Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Electro

Nickel

Plated‐PTFE

Opticote 450

Clear and bright

Fluid clear and

bright, no solids

seen

150.6769 150.6756 4.30 1.06

Everslik 1301 Clear and bright

Fluid clear and

bright, no solids

seen

44.4342 44.4359 ‐1.7 ‐0.42

Everslik 1201

/ 1301 Clear and bright

Fluid clear and

bright, no solids

seen

44.5610 44.5621 ‐1.1 ‐0.27


Fluid clear and

bright, no solids

seen

1.2416 1.2405 1.1 1.75


Fluid clear and

bright, no solids

seen

1.3881 1.3887 ‐0.6 ‐0.79


Fluid clear and

bright, no solids

seen

2.3055 2.3065 ‐1 ‐1.06


Fluid clear and

bright, no solids

seen

2.4051 2.4051 0 0.00


Fluid clear and

bright, no solids

seen

1.5670 1.5666 0.4 0.52


Fluid clear and

bright, no solids

seen

3.4908 3.4913 ‐0.5 ‐0.28

All metals listed conform to the ISO 13628‐6 specification indicating excellent compatibility with

CLEO. Yellow metals show a slight discolouration of the test piece suggesting slight oxidation of

the surface.

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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

138

4.7.2.1.c ‐ CLEO (Neat) Metals Compatibility at 70 °C (12 week data)


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

17 – 4 – PH

UNS

S17400

Clear and bright

Fluid clear and

bright, no solids

seen

99.4731 99.4749 ‐1.8 ‐0.33


Fluid clear and

bright, no solids

seen

9.2972 9.2977 ‐0.50 ‐0.30

A182 F51

UNS

S31803 /

A890 GR4A

(Super

Duplex)

Clear and bright

Fluid clear and

bright, no solids

seen

97.2553 97.2556 ‐0.30 ‐0.06

A182 F53

UNS 32750

(Super

Duplex)

Clear and bright

Fluid clear and

bright, no solids

seen

61.1956 61.1958 0.6 0.15


Fluid clear and

bright, no solids

seen

2.3364 2.3363 0.10 0.00

AISI A29

4340 Gas

Nitrided

Clear and bright

Fluid clear and

bright, no solids

seen

94.9842 94.9847 ‐0.50 ‐0.09

AISI A29


Fluid clear and

bright, no solids

seen

88.2251 88.2253 ‐0.2 ‐0.04

AISI A350

LF2 Carbon

Steel

Clear and bright

Fluid clear and

bright, no solids

seen

95.6857 95.6885 ‐2.80 ‐0.50


Fluid clear and

bright, no solids

seen

123.3737 123.3737 0.00 0.00


Fluid clear and

bright, no solids

seen

123.7503 123.7502 0.10 0.01


Fluid clear and

bright, no solids

seen

160.0036 160.0032 0.40 0.05


Fluid clear and

bright, no solids

seen

161.9419 161.9418 0.1 0.01

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139


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright, no solids

seen

308.42 308.46 ‐40 ‐3.42


Fluid clear and

bright, no solids

seen

96.4047 96.4068 ‐2.10 ‐0.39


Fluid clear and

bright, no solids

seen

156.2514 156.2518 ‐0.4 ‐0.05

Aluminium

Bronze

HM9843

Clear and bright

Fluid clear and

bright, no solids

seen

97.7409 97.7413 1.1 0.22

Aluminium

Bronze UNS

C63000

Slight darkening of

metal.

Fluid clear and

bright, no solids

seen

96.7134 96.7152 ‐1.8 ‐0.34


Fluid clear and

bright, no solids

seen

10.4013 10.4014 ‐0.10 ‐0.05

ASTM B418

Aluminium

Bronze

Clear and bright

Fluid clear and

bright, no solids

seen

87.8577 87.8593 ‐0.8 ‐0.25

Becol

UNS

C17200

Slight darkening of

metal

Fluid clear and

bright, no solids

seen

106.1152 106.116 ‐0.8 ‐0.14

Carbon

Steel UNS

K02401

Clear and bright.

Fluid clear and

bright, no solids

seen

18.0974 18.0978 ‐0.4 ‐0.08

Chrome


Fluid clear and

bright, no solids

seen

3.7174 3.7177 ‐0.30 ‐0.47


Fluid clear and

bright, no solids

seen

49.8892 ‐0.0007 0.4 0.04

CuAl10Ni Minor Staining

Fluid clear and

bright, no solids

seen

8.8022 8.8022 0.00 0.00


Fluid clear and

bright, no solids

seen

4.968 4.9678 0.20 0.11

Duplex


Fluid clear and

bright, no solids

seen

156.5329 156.5328 0.10 0.01

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140


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Electro

Nickel

Plated

Clear and bright

Fluid clear and

bright, no solids

seen

6.9102 6.9101 0.1 0.02


Fluid clear and

bright, no solids

seen

0.9924 0.9924 0.00 0.00


Fluid clear and

bright, no solids

seen

174.7289 174.7309 2.00 0.23


Fluid clear and

bright, no solids

seen

9.6885 9.6886 ‐0.10 ‐0.06

Inconel 718


Fluid clear and

bright, no solids

seen

8.7772 8.7775 ‐0.20 ‐0.13

Inconel 718

Gold

Coated

Clear and bright

Fluid clear and

bright, no solids

seen

0.5725 0.5725 0.00 0.00

Inconel 725


Fluid clear and

bright, no solids

seen

10.3738 10.3742 ‐0.30 ‐0.05

Inconel 725


Fluid clear and

bright, no solids

seen

37.6248 37.6254 ‐0.60 ‐0.35


Fluid clear and

bright, no solids

seen

170.3522 170.3524 ‐0.2 ‐0.02


Fluid clear and

bright, no solids

seen

158.7374 158.7371 0.3 0.04


Fluid clear and

bright, no solids

seen

17.8924 17.8910 1.40 0.43

Mild Steel Trace darkening of

metal

Fluid clear and

bright, no solids

seen

45.2389 45.2395 ‐0.6 ‐0.07

Monel Alloy


Fluid clear and

bright, no solids

seen

149.3270 149.3264 0.60 0.07

Monel Alloy


Fluid clear and

bright, no solids

seen

174.102 174.1006 1.40 0.16


Fluid clear and

bright, no solids

seen

10.0089 9.9897 ‐0.20 ‐0.11

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141


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright, no solids

seen

0.772 0.7718 0.20 0.38

Phosphor

Bronze

PB102

Clear and bright

Fluid clear and

bright, no solids

seen

177.397 177.401 0.1 0.01

Super

Duplex

AM8831

Clear and bright

Fluid clear and

bright, no solids

seen

156.4496 156.454 ‐4.4 ‐0.56

Super

Duplex UNS

S32760

Clear and bright

Fluid clear and

bright, no solids

seen

107.7365 107.74 ‐0.60 ‐0.11

Silicon


Fluid clear and

bright, no solids

seen

3.502 3.5021 ‐0.10 ‐0.26

Stainless


Fluid clear and

bright, no solids

seen

44.4013 44.4024 ‐1.1 ‐0.14

Stainless


Fluid clear and

bright, no solids

seen

55.7968 55.797 ‐0.2 ‐0.04

Stainless


Fluid clear and

bright, no solids

seen

151.314 151.3142 ‐0.20 ‐0.03

Stainless


Fluid clear and

bright, no solids

seen

154.1852 154.1844 0.80 0.11

Super

Duplex

Cameron

Clear and bright

Fluid clear and

bright, no solids

seen

9.1622 9.1625 ‐0.30 ‐0.18


Fluid clear and

bright, no solids

seen

87.7966 87.7968 ‐0.2 ‐0.05

Toughmet 3

AT110 (UNS

C72900)

Copper

Nickel Tin

Alloy, AMS

4596, ASTM

B 929

Clear and bright

(308 AJU)

Fluid clear and

bright, no solids

seen

31.7061 31.7065 0.4 0.10

Clear and bright

(308 ANB)

Fluid clear and

bright, no solids

seen

31.7143 31.7144 0.7 0.18

Clear and bright

(309AAE)

Fluid clear and

bright, no solids

seen

31.657 31.6575 0.3 0.08

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142


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright, no solids

seen

15.7842 15.7846 ‐0.20 ‐0.04


Fluid clear and

bright, no solids

seen

6.524 6.5239 0.10 0.14

Zn plated


Fluid clear and

bright, no solids

seen

5.2813 5.2812 0.10 0.06

6% Ni

Bonded

Tungsten

Carbide

Clear and bright.

Fluid clear and

bright, no solids

seen

11.2051 11.2054 ‐0.3 ‐0.15

10% Ni

Bonded

Tungsten

Carbide

Clear and bright.

Fluid clear and

bright, no solids

seen

11.0026 11.0026 0 0.00

All metals listed have a corrosion rate of less than 0.8 µm per annum after 12 weeks aging at 70 °C

which is an order of magnitude below the limit of 10 µm per annum specified in ISO 13628‐6.

All metals listed conform to the ISO 13628‐6 specification indicating excellent compatibility with

CLEO. Yellow metals show a slight discolouration of the test piece suggesting slight oxidation of

the surface.

Offsh

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143

Coating

Type Appearance of coating

Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Electro

Nickel

Plated‐

PTFE

Opticote

450

Clear and Bright

Fluid clear and

bright, no solids

seen

150.6769 150.6757 1.2 0.15

Everslik

1301 Clear and Bright

Fluid clear and

bright, no solids

seen

44.4342 44.4375 ‐3.3 ‐0.40

Everslik


Fluid clear and

bright, no solids

seen

44.5610 44.5639 ‐2.9 ‐0.36

Xylan 1014 Slight removal of

coating where cut

Fluid clear and

bright, no solids

seen

1.2416 1.2406 1 0.79


Fluid clear and

bright, no solids

seen

1.3881 1.3885 ‐0.4 ‐0.26

Xylan 1212 Clear and Bright

Fluid clear and

bright, no solids

seen

2.3055 2.306 ‐0.5 ‐0.26


Fluid clear and

bright, no solids

seen

2.4051 2.405 0.1 0.00


coating where cut

Fluid clear and

bright, no solids

seen

1.567 1.5668 0.2 0.13


coating where cut

Fluid clear and

bright, no solids

seen

3.4908 3.4908 0 0.00

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144

4.7.2.2.a ‐ CLEO with 10% Sea Water ‐ Metals Compatibility at 70 °C (3 week data)


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

17 – 4 – PH

UNS

S17400

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

99.4931 99.4941 ‐1 ‐0.73


Fluid clear and

bright*.

No Solids Seen.

9.2691 9.2692 ‐0.1 ‐0.24

A182 F51

UNS

S31803 /

A890 GR4A

(Super

Duplex)

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

79.8109 79.8119 ‐1 ‐0.85

A182 F53

UNS 32750

(Super

Duplex)

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

51.311 51.3117 ‐0.7 ‐0.80

AlCNC10 Slight dulling of metal

Fluid clear and

bright*.

No Solids Seen.

2.3447 2.3448 ‐0.1 ‐0.42

AISI A29

4340 Gas

Nitrided

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

94.9837 94.9869 ‐1.9 ‐1.35

AISI A29


Fluid clear and

bright*.

No Solids Seen.

86.0979 86.1005 ‐1.3 ‐0.97

AISI A350

LF2 Carbon

Steel

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

89.9527 89.9559 ‐1.9 ‐1.40


Fluid clear and

bright*.

No Solids Seen.

123.3134 123.31 1.00 0.59


Fluid clear and

bright*.

No Solids Seen.

123.5237 123.52 0.90 0.52


Fluid clear and

bright*.

No Solids Seen.

160.1355 160.13 1.00 0.51


Fluid clear and

bright*.

No Solids Seen.

161.9378 161.9342 3.6 1.84


Fluid clear and

bright*.

No Solids Seen.

308.17 308.18 ‐10 ‐3.42

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ils Ltd.

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

145


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright*.

No Solids Seen.

96.4043 96.4074 ‐1.6 ‐1.19


Fluid clear and

bright*.

No Solids Seen.

157.5122 157.5082 4 2.09

Aluminium

Bronze

HM9843

Slightly dulled

Fluid clear and

bright*.

No Solids Seen.

102.3154 102.3174 ‐0.1 ‐0.08

Aluminium

Bronze UNS

C63000

Slightly dulled

Fluid clear and

bright*.

No Solids Seen.

95.4597 95.461 ‐1.3 ‐0.97

Alloy 3 Slight dulling of metal

Fluid clear and

bright*.

No Solids Seen.

10.2452 10.2455 ‐0.3 ‐0.66

ASTM B418

Aluminium

Bronze

Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

84.7526 84.7536 0.3 0.23

Becol

UNS

C17200

Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

105.3943 105.396 ‐1.7 ‐1.18

Carbon

Steel UNS

K02401

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

18.0146 18.0146 0 0.00

Chrome


Fluid clear and

bright*.

No Solids Seen.

3.7176 3.7179 ‐0.3 ‐1.89

Copper Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

49.5357 49.5344 1.3 0.58


Fluid clear and

bright*.

No Solids Seen.

8.7978 8.7979 ‐0.1 ‐0.22

DGS1043 Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

4.9874 4.9874 0 0.00

Duplex


Fluid clear and

bright*.

No Solids Seen.

156.7245 156.7251 ‐0.6 ‐0.31

Electro

Nickel

Plated

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

6.8225 6.823 ‐0.5 ‐0.04

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ils Ltd.

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

146


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright*.

No Solids Seen.

0.9865 0.9858 0.7 8.92


Fluid clear and

bright*.

No Solids Seen.

174.6883 174.69 0.00 0.00


Fluid clear and

bright*.

No Solids Seen.

9.6388 9.639 ‐0.2 ‐0.47

Inconel 718

Ag Coated

Slight colour change

on metal

Fluid clear and

bright*.

No Solids Seen.

8.7948 8.7954 ‐0.6 ‐1.53

Inconel 718

Gold

Coated

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

0.5905 0.5905 0.00 0.00

Inconel 725


Fluid clear and

bright*.

No Solids Seen.

10.3505 10.3531 ‐2.6 ‐1.73

Inconel 725


Fluid clear and

bright*.

No Solids Seen.

37.4532 37.453 0.2 0.47


Fluid clear and

bright*.

No Solids Seen.

169.5726 169.5751 ‐2.5 ‐1.22


Fluid clear and

bright*.

No Solids Seen.

161.6868 161.6867 0.1 0.05


Fluid clear and

bright*.

No Solids Seen.

17.9608 17.961 ‐0.2 ‐0.25

Monel Alloy


Fluid clear and

bright*.

No Solids Seen.

149.109 149.11 0.50 0.25

Monel Alloy


Fluid clear and

bright*.

No Solids Seen.

174.4189 174.42 0.70 0.32


Fluid clear and

bright*.

No Solids Seen.

9.9911 9.9912 ‐0.1 ‐0.23


Fluid clear and

bright*.

No Solids Seen.

0.7643 0.7647 ‐0.4 ‐3.01

Offsh

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ils Ltd.

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

147


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Phosphor

Bronze

PB102

Slight darkening

Fluid clear and

bright*.

No Solids Seen.

177.4539 177.4518 2.1 0.99

Super

Duplex

AM8831

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

156.5043 156.5065 ‐2.2 ‐1.12

Super

Duplex UNS

S32760

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

105.4411 105.4422 ‐1.1 ‐0.78

Silicon


Fluid clear and

bright*.

No Solids Seen.

3.5002 3.5001 0.1 1.04

Stainless


Fluid clear and

bright*.

No Solids Seen.

48.4503 48.4511 ‐0.8 ‐0.38

Stainless


Fluid clear and

bright*.

No Solids Seen.

56.1237 56.1246 ‐0.9 ‐0.64

Stainless


Fluid clear and

bright*.

No Solids Seen.

151.5104 151.5121 ‐1.7 ‐0.91

Stainless


Fluid clear and

bright*.

No Solids Seen.

154.3478 154.3494 ‐1.6 ‐0.85

Super

Duplex

Cameron

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

9.1230 9.1232 ‐0.2 ‐0.49


Fluid clear and

bright*.

No Solids Seen.

87.6771 87.6774 ‐0.3 ‐0.28

Toughmet 3

AT110 (UNS

C72900)

Copper

Nickel Tin

Alloy, AMS

4596, ASTM

B 929

Annealing Condition

AJU

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

31.6662 31.6665 ‐0.3 ‐0.31

Annealing Condition

ANB

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

31.6739 31.6735 0.4 0.41

Annealing Condition

AAE

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

31.6666 31.6669 ‐0.3 ‐0.31


Fluid clear and

bright*.

No Solids Seen.

13.3904 13.391 ‐0.6 ‐0.50

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ils Ltd.

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ISO 13628‐6 (2012)

148


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright*.

No Solids Seen.

6.5227 6.5228 0 0.00

Zn plated


Fluid clear and

bright*.

No Solids Seen.

5.6096 5.6101 ‐0.5 ‐1.10

6% Ni

Bonded

Tungsten

Carbide

Slightly dulled

Fluid clear and

bright*.

No Solids Seen.

11.2018 11.2021 ‐0.3 ‐0.62

10% Ni

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

11.0431 11.0427 0.4 0.83

Coating


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Everslik


Fluid clear and

bright*.

No Solids Seen.

44.3688 44.3744 ‐5.6 ‐2.74

Everslik

1201 / 1301 Clear and Bright

Fluid clear and

bright*.

No Solids Seen.

44.4864 44.4921 ‐5.7 ‐2.79


Fluid clear and

bright*.

No Solids Seen.

1.4757 1.4755 0.2 0.51


Fluid clear and

bright*.

No Solids Seen.

1.3185 1.3183 0.2 0.51


Fluid clear and

bright*.

No Solids Seen.

2.854 2.8556 ‐1.6 ‐2.85


Fluid clear and

bright*.

No Solids Seen.

2.8184 2.8187 ‐0.3 ‐0.53


coating

Fluid clear and

bright*.

No Solids Seen.

1.2411 1.241 0.1 0.30


coating

Fluid clear and

bright*.

No Solids Seen.

3.4163 3.4191 ‐2.8 ‐4.56

All metals listed conform to the ISO 13628‐6 specification in the presence of 10% sea water

indicating excellent compatibility with CLEO. Yellow metals show a slight discolouration of the test

piece suggesting slight oxidation of the surface.

Offsh

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ils Ltd.

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

149

4.7.2.2.b ‐ CLEO with 10% Sea Water ‐ Metals Compatibility at 70 °C (6 week data)


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

17 – 4 – PH

UNS

S17400

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

99.4931 99.4924 0.7 0.25


Fluid clear and

bright*.

No Solids Seen.

9.2691 9.2691 0 0.00

A182 F51

UNS

S31803 /

A890 GR4A

(Super

Duplex)

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

79.8109 79.8111 ‐0.2 ‐0.08

A182 F53

UNS 32750

(Super

Duplex)

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

51.311 51.311 0 0.00

AlCNC10 Slight dulling of metal

Fluid clear and

bright*.

No Solids Seen.

2.3447 2.3446 0.1 0.21

AISI A29

4340 Gas

Nitrided

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

94.9837 94.9848 ‐1.1 ‐0.39

AISI A29


Fluid clear and

bright*.

No Solids Seen.

86.0979 86.0989 ‐1 ‐0.37

AISI A350

LF2 Carbon

Steel

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

89.9527 89.9541 ‐1.4 ‐0.52


Fluid clear and

bright*.

No Solids Seen.

123.3134 123.3121 1.3 0.38


Fluid clear and

bright*.

No Solids Seen.

123.5237 123.5225 1.2 0.35


Fluid clear and

bright*.

No Solids Seen.

160.1355 160.1344 1.1 0.28


Fluid clear and

bright*.

No Solids Seen.

161.9378 161.9373 0.5 0.13

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vironmental O

ils Ltd.

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

150


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright*.

No Solids Seen.

308.17 308.41 ‐20 ‐3.42


Fluid clear and

bright*.

No Solids Seen.

96.4043 96.4052 ‐0.9 ‐0.34


Fluid clear and

bright*.

No Solids Seen.

157.5122 157.512 0.2 0.05

Aluminium

Bronze

HM9843

Slightly dulled metal

Fluid clear and

bright*.

No Solids Seen.

102.3101 102.3095 0.6 0.24

Aluminium

Bronze UNS

C63000

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

95.4597 95.4598 ‐0.1 ‐0.04

Alloy 3 Slight dulling of metal

Fluid clear and

bright*.

No Solids Seen.

10.2452 10.2454 ‐0.3 ‐0.33

ASTM B418

Aluminium

Bronze

Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

84.7526 84.7512 1.4 0.53

Becol

UNS

C17200

Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

105.3943 105.3953 ‐1 ‐0.35

Carbon

Steel UNS

K02401

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

18.0146 0.3 0.3 0.11

Chrome


Fluid clear and

bright*.

No Solids Seen.

3.7176 3.7175 0.1 0.32

Copper Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

49.5357 49.5324 0.1 0.02


Fluid clear and

bright*.

No Solids Seen.

8.7978 8.7976 0.2 0.22

DGS1043 Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

4.9874 4.9871 0.4 0.45

Duplex


Fluid clear and

bright*.

No Solids Seen.

156.7245 156.7255 ‐1 ‐0.26

Offsh

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ils Ltd.

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

151


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Electro

Nickel

Plated

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

6.8225 6.8227 ‐0.2 ‐0.09


Fluid clear and

bright*.

No Solids Seen.

0.9865 0.9865 0 0.00


Fluid clear and

bright*.

No Solids Seen.

174.6883 174.6879 0.4 0.09


Fluid clear and

bright*.

No Solids Seen.

9.6388 9.6388 0 0.00

Inconel 718

Ag Coated


on metal

Fluid clear and

bright*.

No Solids Seen.

8.7948 8.7939 0.9 1.15

Inconel 725

GV50H


on metal

Fluid clear and

bright*.

No Solids Seen.

10.3505 10.3525 ‐1.9 ‐0.63

Inconel 725


Fluid clear and

bright*.

No Solids Seen.

37.4532 37.4523 0.9 1.05

Inconel 718

Gold Plated Clear and bright

Fluid clear and

bright*.

No Solids Seen.

0.5677 0.5677 0.00 0.00


Fluid clear and

bright*.

No Solids Seen.

169.5726 169.5736 ‐1 ‐0.24


Fluid clear and

bright*.

No Solids Seen.

161.6868 161.687 ‐0.2 ‐0.05


Fluid clear and

bright*.

No Solids Seen.

17.9608 17.9607 0.1 0.06

Monel Alloy


Fluid clear and

bright*.

No Solids Seen.

149.109 149.1084 0.6 0.15

Monel Alloy


Fluid clear and

bright*.

No Solids Seen.

174.4189 174.4178 1.1 0.25


Fluid clear and

bright*.

No Solids Seen.

9.9911 9.9911 ‐0.1 ‐0.11


Fluid clear and

bright*.

No Solids Seen.

0.7643 0.7643 0 0.00

Offsh

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ils Ltd.

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

152


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Phosphor

Bronze

PB102

Slight staining of

metal

Fluid clear and

bright*.

No Solids Seen.

176.75 176.7512 ‐1.2 ‐0.28

Super

Duplex

AM8831

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

156.5043 156.5044 ‐0.1 ‐0.03

Super

Duplex UNS

S32760

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

105.4411 105.4397 1.4 0.50

Silicon


Fluid clear and

bright*.

No Solids Seen.

3.5002 3.5001 0.1 0.52

Stainless


Fluid clear and

bright*.

No Solids Seen.

48.4503 48.4512 ‐0.9 ‐0.22

Stainless


Fluid clear and

bright*.

No Solids Seen.

56.1237 56.1239 ‐0.2 ‐0.07

Stainless


Fluid clear and

bright*.

No Solids Seen.

151.5104 151.5107 ‐0.3 ‐0.08

Stainless


Fluid clear and

bright*.

No Solids Seen.

154.3478 154.3484 ‐0.6 ‐0.16

Super

Duplex

Cameron

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

9.1230 9.1228 0.2 0.25


Fluid clear and

bright*.

No Solids Seen.

87.6771 87.6777 ‐0.6 ‐0.28

Toughmet 3

AT110 (UNS

C72900)

Copper

Nickel Tin

Alloy, AMS

4596, ASTM

B 929

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

31.6662 31.6658 0.4 0.21

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

31.6739 31.6729 1 0.51

Annealing Condition

AAE

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

31.6666 31.6662 0.4 0.21

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ils Ltd.

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

153


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright*.

No Solids Seen.

13.3904 13.3906 ‐0.4 ‐0.17


Fluid clear and

bright*.

No Solids Seen.

6.5227 6.5226 0.1 0.28

Zn plated


Fluid clear and

bright*.

No Solids Seen.

5.6096 5.6094 0.2 0.22

6% Ni

Bonded

Tungsten

Carbide

Slightly dulled

Fluid clear and

bright*.

No Solids Seen

11.2018 11.202 ‐0.2 ‐0.21

10% Ni

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

11.0431 11.0429 0.2 0.21

Offsh

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ils Ltd.

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

154

Coating


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Everslik


Fluid clear and

bright*.

No Solids Seen.

44.3688 44.3746 ‐5.8 ‐1.42

Everslik

1201 / 1301 Clear and Bright

Fluid clear and

bright*.

No Solids Seen.

44.4864 44.4933 ‐6.9 ‐1.69


Fluid clear and

bright*.

No Solids Seen.

1.4757 1.4755 0.2 0.25


Fluid clear and

bright*.

No Solids Seen.

1.3185 1.3182 0.3 0.38


Fluid clear and

bright*.

No Solids Seen.

2.854 2.855 ‐1 ‐0.89


Fluid clear and

bright*.

No Solids Seen.

2.8184 2.8188 ‐0.4 ‐0.35


coating

Fluid clear and

bright*.

No Solids Seen.

1.2411 1.2410 0.1 0.15


coating

Fluid clear and

bright*.

No Solids Seen.

3.4163 3.4241 ‐7.8 ‐6.35

All metals listed conform to the ISO 13628‐6 specification in the presence of 10% sea water

indicating excellent compatibility with CLEO. Yellow metals show a slight discolouration of the test

piece suggesting slight oxidation of the surface.

Offsh

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vironmental O

ils Ltd.

TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

155

4.7.2.2.c ‐ CLEO with 10% Sea Water ‐ Metals Compatibility at 70 °C (12 week data)


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

17 – 4 – PH

UNS

S17400

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

99.4931 99.4947 ‐1.6 ‐0.29


Fluid clear and

bright*.

No Solids Seen.

9.2691 9.2691 0.1 0.06

A182 F51

UNS

S31803 /

A890 GR4A

(Super

Duplex)

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

79.8109 79.8134 ‐2.5 ‐0.53

A182 F53

UNS 32750

(Super

Duplex)

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

51.311 51.3119 ‐0.9 ‐0.26

AlCNC10 Slightly dulled metal

Fluid clear and

bright*.

No Solids Seen

2.3447 2.3446 0.1 0.11

AISI A29

4340 Gas

Nitrided

Clear and bright

Fluid clear and

bright*.

No Solids Seen

94.9837 94.9855 ‐1.8 ‐0.32

AISI A29


Fluid clear and

bright*.

No Solids Seen

86.0979 86.0994 ‐1.5 ‐0.28

AISI A350

LF2 Carbon

Steel

Clear and bright

Fluid clear and

bright*.

No Solids Seen

89.9527 89.9544 ‐1.7 ‐0.31


Fluid clear and

bright*.

No Solids Seen.

123.3134 123.31 1.30 0.19


Fluid clear and

bright*.

No Solids Seen.

123.5237 123.52 1.10 0.16


Fluid clear and

bright*.

No Solids Seen.

160.0057 160.01 0.50 0.06

AISI 1040 Clear and bright Fluid clear and

bright*.

No Solids Seen

161.9378 161.9364 1.4 0.18

Offsh

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TECHNICAL MANUAL TO

ISO 13628‐6 (2012)

156


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright*.

No Solids Seen

308.17 308.58 ‐40 ‐3.42


bright*.

No Solids Seen

96.4043 96.4059 ‐1.6 ‐0.30


bright*.

No Solids Seen

157.5122 157.5109 1.3 0.17

Aluminium

Bronze

HM9843

Dulling of metal.

Fluid clear and

bright*.

No Solids Seen.

102.3101 102.3111 ‐1 ‐0.20

Aluminium

Bronze UNS

C63000

Dulling of metal

Fluid clear and

bright*.

No Solids Seen.

95.4597 95.4609 ‐1.2 ‐0.22

Alloy 3 Darkening of metal Fluid clear and

bright*.

No Solids Seen.

10.2452 10.2453 ‐0.2 ‐0.11

ASTM B418

Aluminium

Bronze

Slight darkening of

metal.

Fluid clear and

bright*.

No Solids Seen.

84.7526 84.751 1.6 0.31

Becol

UNS

C17200

Slight darkening of

metal

Fluid clear and

bright*.

No Solids Seen.

105.3943 105.3947 ‐0.4 ‐0.07

Carbon

Steel UNS

K02401

Clear and bright, light

markings were

spacers contacted.

Fluid clear and

bright*.

No Solids Seen.

18.1016 18.102 ‐0.4 ‐0.08

Chrome

Core Clear and bright.

Fluid clear and

bright*.

No Solids Seen.

3.7176 3.7175 0.1 0.16

Copper Darkening of metal

Fluid clear and

bright*.

No Solids Seen.

49.5357 49.5309 4.8 0.53

CuAl10Ni Minor staining. Fluid clear and

bright*.

No Solids Seen.

8.7978 8.7976 0.2 0.11

DGS1043 Moderate staining.

Fluid clear and

bright*.

No Solids Seen.

4.9874 4.9871 0.4 0.22

Duplex

9490 Clear and bright.

Fluid clear and

bright*.

No Solids Seen.

156.7245 156.7282 ‐3.7 ‐0.48

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Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Electro

Nickel

Plated

Clear and bright.

Fluid clear and

bright*.

No Solids Seen

6.8225 6.8222 0.3 0.06

Elgiloy Clear and bright.

Fluid clear and

bright*.

No Solids Seen.

0.9865 0.9865 0 0.00

Inconel 625 Clear and bright.

Fluid clear and

bright*.

No Solids Seen.

174.6883 174.69 0.20 0.02


Fluid clear and

bright*.

No Solids Seen.

9.6388 9.6388 0 0.00

Inconel 718

Ag Coated Minor colouration.

Fluid clear and

bright*.

No Solids Seen.

8.7948 8.794 0.8 0.51

Inconel 718

Gold

Coated

Clear and bright.

Fluid clear and

bright*.

No Solids Seen.

0.5534 0.5534 0 0.00

Inconel 725

GV50H Clear and bright.

Fluid clear and

bright*.

No Solids Seen.

10.3505 10.3527 ‐2.1 ‐0.35

Inconel 725

Ag Coated Minor colouration.

Fluid clear and

bright*.

No Solids Seen.

37.4532 37.4523 0.9 0.52


Fluid clear and

bright*.

No Solids Seen.

169.5726 169.5675 5.1 0.62


Fluid clear and

bright*.

No Solids Seen.

161.6868 161.6866 0.2 0.03

KR16 Clear and bright.

Fluid clear and

bright*.

No Solids Seen.

17.9608 17.9609 0.1 0.03

Monel Alloy


Fluid clear and

bright*.

No Solids Seen.

149.109 149.11 0.50 0.06

Monel Alloy

K500 Clear and bright.

Fluid clear and

bright*.

No Solids Seen.

174.4189 174.42 0.60 0.07

MP35N Clear and bright.

Fluid clear and

bright*.

No Solids Seen.

9.9911 9.9911 ‐0.1 ‐0.06


Fluid clear and

bright*.

No Solids Seen.

0.7643 0.7641 0.2 0.38

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Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Phosphor

Bronze

PB102

Dulling of metal

Fluid clear and

bright*.

No Solids Seen.

176.75 176.7528 ‐2.8 ‐0.33

Super

Duplex

AM8831

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

156.5043 156.5077 ‐3.4 ‐0.43

Super

Duplex UNS

S32760

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

105.4411 105.4392 1.9 0.34

Silicon


Fluid clear and

bright*.

No Solids Seen.

3.5002 3.5 0.2 0.52

Stainless


Fluid clear and

bright*.

No Solids Seen.

48.4503 48.4521 ‐1.8 ‐0.22

Stainless


Fluid clear and

bright*.

No Solids Seen.

56.1237 56.1249 ‐1.2 ‐0.21

Stainless


Fluid clear and

bright*.

No Solids Seen.

151.5104 151.5156 ‐5.2 ‐0.70

Stainless


Fluid clear and

bright*.

No Solids Seen.

154.3478 154.3517 ‐3.9 ‐0.52

Super

Duplex

Cameron

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

9.1230 9.1229 0.1 0.06


Fluid clear and

bright*.

No Solids Seen.

87.6771 87.6803 ‐3.2 ‐0.75

Toughmet 3

AT110 (UNS

C72900)

Copper

Nickel Tin

Alloy, AMS

4596, ASTM

B 929

Annealing Condition

AJU

Slightly dulled.

Fluid clear and

bright*.

No Solids Seen.

31.6662 31.6651 1.1 0.28

Annealing Condition

ANB

Slightly dulled

Fluid clear and

bright*.

No Solids Seen.

31.6739 31.6726 1.3 0.33

Annealing Condition

AAE

Slightly dulled

Fluid clear and

bright*.

No Solids Seen.

31.6666 31.6655 1.1 0.28

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Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)


Fluid clear and

bright*.

No Solids Seen.

13.3904 13.3905 ‐0.3 ‐0.06


Fluid clear and

bright*.

No Solids Seen.

6.5227 6.5224 0.3 0.42

Zn plated


Fluid clear and

bright*.

No Solids Seen.

5.6096 5.6093 0.3 0.16

6% Ni

Bonded

Tungsten

Carbide

Slightly dulled

Fluid clear and

bright*.

No Solids Seen.

11.2018 11.2021 ‐0.3 ‐0.15

10% Ni

Bonded

Tungsten

Carbide

Clear and bright

Fluid clear and

bright*.

No Solids Seen.

11.0431 11.0429 0.2 0.10

All metals listed aged at 70 °C pass the ISO 13628‐6 specification indicating excellent compatibility

with CLEO. Yellow metals have a slight discolouration of the test piece suggesting slight oxidation

of the surface.

All metals listed have a corrosion rate of less than 0.8 µm per annum after 12 weeks aging at 70 °C

which is an order of magnitude below the limit of 10 µm per annum specified in ISO 13628‐6.

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Coating


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Everslik


Fluid clear and

bright*.

No Solids Seen.

44.3688 44.3762 ‐7.4 ‐0.91

Everslik

1201/1301 Clear and bright

Fluid clear and

bright*.

No Solids Seen.

44.4864 44.4971 ‐10.7 ‐1.31


Fluid clear and

bright*.

No Solids Seen.

1.4757 1.4754 0.3 0.19


Fluid clear and

bright*.

No Solids Seen.

1.3185 1.3185 0 0.00

Xylan 1212 Clear and bright Fluid clear and

bright*.

No Solids Seen.

2.854 2.8549 ‐0.9 ‐0.40

Xylan 1213 Clear and bright Fluid clear and

bright*.

No Solids Seen.

2.8184 2.8186 ‐0.2 ‐0.09


coating

Fluid clear and

bright*.

No Solids Seen.

1.2411 1.2412 ‐0.1 ‐0.08

Xylan 1424 Slight bubbling of

coating seen.

Fluid clear and

bright*.

No Solids Seen.

3.4163 3.4346 ‐18.3 ‐7.45

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4.7.3 ‐ AISI 316 Compatibility with Production Control Fluid and 10% Natural Sea Water

Tests are carried out in the neat fluid and aged for 3 weeks, 6 weeks and 12 weeks following the

methodology laid out in ISO 16328‐6 Annex C Protocol with the following deviations / extensions.

The test pieces were aged at 70 °C, which is more severe than the 60 °C testing required

in ISO 13628‐6




samples;




PROCEDURE

The ready‐made metal samples, which have a standard surface area and a standard surface

condition, are degreased, dried and weighed to the nearest 0.1 mg and then immersed in both

the neat control fluid, and in the presence of 10% sea water. It should be noted that when sea

water is present, the metal is exposed completely in the control fluid phase and not the sea water

phase.

Tests were carried out in glass vessels at 70 °C. Nine replicate specimens are exposed in a single

container, with three replicates are retrieved from the fluid after 3 weeks, 6 weeks and 12 weeks.

After visual inspection of the samples and after appropriate cleaning, weight loss is measured and

the samples inspected for visible corrosion attacks, which are characterized. The weight losses are

transcribed into uniform corrosion, in micrometers per year, and maximum depth of local attacks,

in micrometers, is determined under a microscope with a calibrated depth of focus. The fluid is

inspected for any separations, including solid particles or sludge. In addition examination and

characterization with respect to SRP activity before and after the test is carried out.

ACCEPTANCE CRITERIA

No substantial visible corrosion products or attacks on any of the metals,


period,




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RESULTS

The results for CLEO as a function of time are shown below indicate that all the test pieces passed

the ISO 13628‐6 specification.

Aging Time /

weeks Appearance of metal

Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per

annum)

SRP

Activity

3 weeks

Clear

and

bright

Fluid clear and

bright*.

No Solids Seen.

127.295 127.296

7 ‐1.7 ‐0.98

None 127.1968 127.198

1 ‐1.3 ‐0.75

127.3655 127.366

8 ‐1.3 ‐0.75

6 weeks

Clear

and

bright

Fluid clear and

bright*.

No Solids Seen.

127.2618 127.264

3 ‐2.5 ‐0.72

None

127.3533 127.356

1 ‐2.8 ‐0.81

127.1063 127.108

4 ‐2.1 ‐0.60

12 weeks

Clear

and

bright

Fluid clear and

bright*.

No Solids Seen.

127.2712 127.274 ‐2.8 ‐0.37

None 127.1616 127.164

6 ‐3 ‐0.40

127.4666 127.469 ‐2.4 ‐0.32

The results show that CLEO meets the acceptance criteria in ISO 13628‐6 for metal compatibility

with Stainless Steel 316 with 10% Natural Sea Water at 70 °C for 12 weeks.

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4.7.4 – Metal Compatibility at 250 °C


Tests are carried out in the neat fluid and aged for 2 and 6 months following the methodology laid

out in ISO 13628‐6.




samples;




Test at maximum temperature plus 10 °C (18 °F) is carried out in a suitable autoclave made of AISI

316 or better quality material, preferentially lined by PTFE, pressurised to an appropriate level to

prevent boiling (depends on the test temperature). Both materials (AISI 316 and AISI 17‐4 PH,

both with crevice) are exposed in triplicate for each testing period. The test is run for 2 months, 6

months and 12 months in a separate vessel for each testing period. At the termination of the test

the same procedure as for section 2.2 is followed. The results are reported for approval after 6

months.

For synthetic oil based fluids: For the high temperature tests, AISI 316 shall be exposed to the

control fluid and the seawater. 17‐4PH shall only be exposed to the control fluid. Both sets of

metal samples can be exposed in the same container. The vessel should not be purged with

nitrogen before pressurisation, in order to maintain atmospheric air in the vessel.

ACCEPTANCE CRITERIA

No substantial visible corrosion products or attacks on any of the metals.


period.


Corrosion rate of the carbon steel including galvanic coupling shall not exceed 10 μm/year

(12 weeks result).



Corrosion rate of 17‐4PH shall not exceed 5 μm/year (12 weeks result) and maximum


Corrosion rate of electroless nickel shall not exceed 2 µm/year (12 weeks result).

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4.7.4.a – CLEO (Neat) Metal Compatibility at 250 °C (2 Month Data)


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

17 – 4 – PH

(UNS

S17400)

Clear and bright.

None 99.6751 99.6630 12.1 3.05

Clear and bright.

None 99.6929 99.6853 7.6 1.92

Clear and bright.

None 99.8844 99.8749 9.5 2.40

Stainless

Steel 316

Clear and bright.

None 94.4419 94.4418 0.1 0.02

Clear and bright.

None 95.4901 95.4898 0.3 0.07

Clear and bright.

None 96.2700 96.2698 0.2 0.05

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4.7.4.b ‐ CLEO (Neat) Metal Compatibility at 250 °C (6 Month Data)


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

17 – 4 – PH

(UNS

S17400)

Dulled, slight black

surface deposits.

None 99.7460 99.73760 8.4 0.71


surface deposits.

None 99.9326 99.92800 4.6 0.39


surface deposits.

None 99.5411 99.53000 11.1 0.93

Stainless

Steel 316

Clear and bright.

None 22.5269 22.5267 0.2 0.03

Clear and bright.

None 22.5349 22.5346 0.3 0.05

Clear and bright.

None 22.3639 22.3638 0.1 0.02

The results show CLEO meets all the acceptance criteria laid down in ISO 13628‐6 with respect to

metal compatibility at 250 °C for compatibility with Stainless Steel grade 316. The 17‐4‐PH (UNS

S17100) material is showing slight deposits upon extended aging at these elevated temperatures.

Offshore Environmental Oils do not recommend the use of either of these materials at such

elevated temperatures, particularly if the ingress of sea water is likely.

It is generally not recommended that 17‐4‐PH (UNS S17400) or Stainless Steel AISI 316 are used

at such high temperatures in the field with sea water present and that more suitable materials are

selected for field operation at such elevated temperatures.

As a result, we do not recommend the use of Stainless Steel AISI 316 or 17‐4‐PH materials at such

elevated temperatures in the field, particularly if the ingress of sea water is likely. It is also our

opinion that the use of Stainless Steel AISI 316 and 17‐4‐PH within the ISO specification at

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elevated temperatures should be reconsidered in light of the new higher temperatures reached

by CLEO.

4.7.5 – Additional Metal compatibility at 250 °C


Tests are carried out in the neat fluid and aged for 3 weeks, 6 weeks and 12 weeks and are based

on the methodology laid out in ISO 16328‐6 Annex C Protocol for water based subsea fluids

(without sea water) as outlined in section 4.7.1 with the following deviations / extensions.

The test pieces were aged at 250 °C.

Single test pieces only were used as indicated.

Testing in the neat fluid alone was undertaken.

Further testing after 18 weeks aging is also reported, with further testing on‐going.

ACCEPTANCE CRITERIA

No substantial visible corrosion products or attacks on any of the metals.


period.


Corrosion rate of AISI 316 shall not exceed 5 μm/year (6 months result) and maximum


Corrosion rate of 17‐4 PH shall not exceed 5 μm/year (6 months result) and maximum


RESULTS

The results for CLEO are shown overleaf.

Whilst the materials below show excellent compatibility at 250 °C within the fluid, this is not a

recommendation on suitable materials for use at this temperature, rather a demonstration that

the fluid has excellent corrosion protection abilities. For projects operating at such severe

temperatures, careful material selection is advisable based on operational requirements.

All metals tested have a corrosion rate of less than 2 µm per annum after 12 weeks aging at 250

°C which is an order of magnitude below the limit of 10 µm per annum specified in ISO 13628‐6.

Extended testing for these materials is currently on going, and will be expanded to include other

metals in future.

Materials currently on test include:‐

Inconel 625 Inconel 718 Inconel 725 GV50H Inconel 825

Monel Alloy 400 Monel Alloy K500 MP35N Nitronic 50

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Stainless Steel 316 Ti Super Duplex UNS S31803 Super Duplex UNS S32750 Super Duplex UNS S32650

CLEO aged at 250 °C for 3 weeks


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Aluminium

Bronze

(UNS

C63000)

Slight darkening Slightly darkened,

no solids seen 95.1396 95.1391 0.5 0.37

Becol (UNS

C17200) Slight dulling

Slightly darkened,

no solids seen 105.9809 105.9853 ‐4.4 ‐3.07

Stainless


Slightly darkened,

no solids seen 48.7893 48.7893 0 0.00



Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Aluminium

Bronze

(UNS

C63000)


no solids seen 95.1396 95.1394 0.2 0.07

Becol (UNS


Slightly darkened,

no solids seen 105.9809 105.9856 ‐4.7 ‐1.64

Stainless


Slightly darkened,

no solids seen 48.7893 48.7892 0.1 0.02



Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Aluminium

Bronze

(UNS

C63000)


no solids seen 95.1396 95.1383 1.3 0.24

Becol (UNS


Slightly darkened,

no solids seen 105.9809 105.9888 ‐7.9 ‐1.38

Stainless


Slightly darkened,

no solids seen 48.7893 48.7893 0 0.00

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Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Aluminium

Bronze

(UNS

C63000)


no solids seen 95.1396 95.14 3.50 0.43

Becol (UNS


Slightly darkened,

no solids seen 105.9809 105.989 ‐8.1 ‐0.94

Stainless


Slightly darkened,

no solids seen 48.7893 48.7893 0 0.00



Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Aluminium

Bronze

(UNS

C63000)


no solids seen 95.1396 95.1272 12.4 1.24

Becol (UNS


Slightly darkened,

no solids seen 105.9809 105.9816 ‐0.7 ‐0.07

Stainless


Slightly darkened,

no solids seen 48.7893 48.7874 1.9 0.12

CLEO aged at 250 °C for 6 months (26 weeks)


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Aluminium

Bronze

(UNS

C63000)


no solids seen 95.1396 95.1258 13.8 1.17

Becol (UNS


Slightly darkened,

no solids seen 105.9809 105.9832 ‐2.3 ‐0.18

Stainless


Slightly darkened,

no solids seen 48.7893 48.7874 1.9 0.10

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4.7.6 –CLEO with 10% Sea Water Metal Compatibility at 250 °C


Appearance of

fluid (solids /

sludge)

Initial

Weight /

g

Aged

Weight /

g

Weight

Loss /

mg

Corrosion

rate (µm

per annum)

Stainless

Steel 316

Black deposits on

metal as recovered,

heavily dulled metal

after brushing and

chemical cleaning.

Dark brown oil

phase, clear and

bright sea water

phase. Black

deposits in fluid.

22.5346 21.5877 946.9 154.66

Black deposits on

metal as recovered,


after brushing and

chemical cleaning.

Dark brown oil

phase, clear and

bright sea water

phase. Black

deposits in fluid.

22.5189 21.5554 963.5 157.38

Black deposits on

metal as recovered,


after brushing and

chemical cleaning.

Dark brown oil

phase, clear and

bright sea water

phase. Black

deposits in fluid.

22.3921 21.3939 998.2 163.04

It should be noted that Monel K500 autoclaves were used for the tests containing sea water, as

stainless steel 316 is not deemed resistant to sea water at the temperatures involved (250 °C).

The 17‐4‐PH (UNS S17400) material as also omitted from the sea water test as it was found not to

be corrosion resistant to sea water at 250 °C.

The stainless steel 316 pieces were approximately 40 ‐ 50% covered in sea water in these test, and

further testing is planned with the test pieces immersed only in the oil phase in the presence of

sea water at 250 °C.

Further results will be available in Q2 2013 but it is generally not recommended that 17‐4‐PH

(UNS S17400) or AISI 316 are used at such high temperatures in the field with seawater present

and that more suitable materials are selected for field operation at such elevated applications.

As a result, we do not recommend the use of Stainless Steel 316 or 17‐4‐PH materials at such

elevated temperatures in the particularly if the ingress of sea water is likely.

It is also our opinion that the use of Stainless Steel 316 and 17‐4‐PH within the ISO specification at

elevated temperatures should be reconsidered in light of the new higher temperatures reached

by CLEO.

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4.8 – Elastomer Compatibility

4.8.1 – Elastomer Compatibility


Tests are carried out in the neat fluid at a moderate [70°C (158°F)] and high temperature

[maximum plus 10°C (18°F)], respectively. Standard test materials are used, the type depending

on the temperature:

At 70°C (158°F): HNBR 90 (Parker N3512‐90, Skega 63‐90‐093, BusakShamban H9T40), Viton

(Parker V0747), NBR 70 (Parker N‐064‐70, Skega 63‐80‐001, BusakShamban N762A).

At high temperature: PTFE, PEEK, Perfluoroelastomer 90 and HNBR 90 (Parker N3512‐90 Skega

63‐90‐093, BusakShamban H9T40) up to 120oC (248°F).

The following methods are used:

Visual inspection of fluid

Macro‐ and microscopic inspection of the test materials

Volume change for materials

Weight change

Hardness change (Shore A or D) for materials.

PROCEDURE

The procedure is based upon ASTM D471 without tensile testing.

The test specimens are weighed in air and in water and the Shore A or D hardness is measured.

At 70°C (158°F) and the maximum temperature plus 10 °C, three replicate samples are exposed in

the fluid. A separate vessel is used for each material. The same samples are by re‐exposure used

for the exposure periods of 1 week, 1 month and 3 months, respectively. Volume change, weight

change and change in hardness are measured for each sample after each testing period. At the

termination of the test, the test specimens are also investigated with respect to change in

appearance and formation of cracks.

ACCEPTANCE CRITERIA

No visible effect of the tested polymers on the appearance of the fluid.

The appearance of the polymer materials shall not change during the test (some staining

by the fluid is permitted for materials which tend to discolour).

Volume change shall not exceed the range ‐5 % to 10 % at either temperature.

Hardness change shall not exceed 10 % at either temperature.

The development in volume and hardness change with time shall show a clear tendency

to stabilization.

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RESULTS

Results from up to 3 months to date are outlined below.

All elastomers tested in CLEO conform to the ISO 13628‐6 specification after either 1 or 3 months.

Testing for materials which have not yet completed 3 months are currently on going.

CLEO showed excellent compatibility with a wide range of elastomers.

SUMMARY OF ELASTOMER RESULTS

The following elastomers have completed 3 months aging @ 70 °C in accordance with ISO 13628‐6.

Elastomer CLEO

ISO 13628‐6 Comments

Aflas (Clwyd) Pass

Chemraz 510 (Gren Tweed) Pass

Ducoflex Hose Grade 350‐13‐33‐06T Pass

Ecoflon 4 25% Carbon Filled PTFE (Economos) Pass

Elastolion 101 HNBR (James Walker) Pass

FFKM PFR06HC 90 Shore A (Solvay) Pass

FFKM PKR95HT 90 Shore A (Solvay) Pass

FKM 70.16‐14 (Angst and Pfister) Pass

FKM FOR 3752 (Solvay) Pass

FKM FOR 9381 92 Shore A (Solvay) Pass

FKM FR58‐90 James Walker Pass

FKM Mix 80 (FCH) Pass

FKM NT 80.7‐70 (Angst and Pfister) Pass

FKM P757 92 Shore A (Solvay) Pass

FKM P959 93 Shore A (Solvay) Pass

FKM PL855 91 Shore A (Solvay) Pass

FKM VBR X856 90 Shore A (Clwyd) Pass

FKM V70GA 70 Shore A (Trelleborg) Pass

FKM V75J Shore 75 A(Precision Polymer Engineering)

Pass

FKM VPL85540 92 Shore A (Solvay) Pass

FKM VPL 85730 91 Shore A (Solvay) Pass

FKM PL958 91 Shore A (Solvay) Pass

FKM V1238‐95 95 A (Parker) Pass

Flourel (Parker) Pass

HNBR 2269‐90 (Parco) Pass

HNBR 4007 90 Shore A (Parker) Pass

HNBR KB163 90 Shore A (Parker) Pass

HNBR 453702 90 Shore A (Freudenberg) Pass

HNBR H9T40 90 Shore A (Trelleborg) Pass

Hytrel 5556 Shore 55D Thermoplastic Polyester (Dupont) Pass

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Elastomer CLEO


Hytrel 6356 Shore 63D Thermoplastic Polyester (Dupont) Pass

LNP‐PDX 82429 Carbon Filled Teflon (OEM) Pass

NBR K09G 90 Shore A (Pimseal) Pass

NBR N107‐90 (Parker) Pass


NBR N552‐90 90 Shore A (Parker) Pass

NBR N674‐70 70 Shore A (Parker) Pass




NBR N7003 70 Shore A (Trelleborg) Pass




NBR PB80 80 Shore A (James Walker) Pass

NBR N9002‐90 Shore A (Trelleborg) Pass

NBR 70 (Ramsey Services) Pass

NBR70 K6 (GAPI Compounds) Pass

NBR 70 (Eriks Seals) Pass

Nylon 6 (Skiffy) Pass

Nylon TLO (OEM) Pass

Nylon XLPE (OEM) Pass

PEEK 450G (Victrex) Pass

PEEK 450CA30 (30% Carbon Filled) (Victrex) Pass

PEEK 1000 (OEM) Pass

PEEK W4685 (Parker) Pass

PEEK W4738 (Parker) Pass

Polyamide Imide AMS 3670‐1 (OEM) Pass

Polyamide Imide AMS 3670‐4 (OEM) Pass

Polyurethane (OEM) Pass

POM (polyoxymethylene) (OEM) Pass

PTFE (OEM) Pass

PTFE (25% Carbon Filled) (OEM) Pass

PTKC (OEM) Pass

PVDF (OEM) Pass

Turcon T19 (Trelleborg) Pass

Turcon T29 Step Seal (Trelleborg) Pass



Viton 70 (OEM) Pass

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Elastomer CLEO


Viton 90 (OEM) Pass

Viton A 9009‐75 (OEM) Pass

Viton Extreme 90 Shore A (Clwyd) Pass

Viton HTV90‐A2 90 Shore A (Dupont) Pass

Viton V747‐75 (Parker) Pass

Zurcon Z25 95 Shore A (Trelleborg) Pass

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Elastomer Compatibility with CLEO at 70 °C

Elastomer (Supplier)

Aging Time

Fluid Appearance Median Swell

Change %

Median Loss of Shore

Hardness % ISO 13628‐6

Aflas (Clwyd)

1 week Clear and bright 0.30 9.70

Pass 1 month Clear and bright 0.40 9.70

3 months Clear and bright 0.60 9.90

Chemraz 510 (Green Tweed)




Ducoflex Hose Grade 350‐13‐33‐06T (Duco)




Ecoflon 4 25% Carbon Filled PTFE

(Economos)




Elastolion 101 HNBR

(James Walker)




FFKM PFR06HC 90 Shore A (Solvay)




FFKM PKR95HT 90 Shore A

(Solvay)




FKM 70.16‐14 (Angst and Pfister)




FKM FOR 3752 (Solvay)




FKM FOR 9381 92 Shore A (Solvay)




FKM FR58‐90 James Walker




FKM Mix 80 (FCH)




FKM NT 80.7.70 (Angst and Pfister)




FKM P757 92 Shore A (Solvay)




FKM P959 93 Shore A (Solvay)




FKM PL855 91 Shore A (Solvay)




FKM VBR X856 90 Shore A (Clwyd)




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Elastomer Compatibility with CLEO at 70 °C (cont.)


Aging Time


Change %



FKM VPL85540 92 Shore A (Solvay)




FKM VPL 85730 91 Shore A

(Solvay)




FKM PL958 91 Shore A (Solvay)




FKM V1238‐95 95 Shore A (Parker)




Flourel (Parker)




HNBR 2269‐90 (Parco)




HNBR 4007 90 Shore A (Parker)




HNBR KB163 90 Shore A (Parker)




HNBR 453702 90 Shore A (Freudenberg)




HNBR H9T40 90 Shore A

(Trelleborg)




Hytrel 5556 Shore 55D Thermoplastic Polyester

(Dupont)




Hytrel 6356 Shore 63D Thermoplastic Polyester

(Dupont)




Lnp‐pdx 82429 Carbon Filled Teflon (OEM)




NBR K09G 90 Shore A (Pimseal)




NBR N107‐90 (Parker)








NBR N552‐90 90 Shore A (Parker)




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Aging Time


Change %



NBR N674‐70 70 Shore A (Parker)








NBR N1059‐90 (Parker




NBR N1444‐90 (Parker




NBR N7003 70 Shore A (Trelleborg)




NBR N7022 70 Shore A

(Trelleborg)





(Trelleborg)





(Trelleborg)




NBR N9002 90 Shore A (Trelleborg)




NBR PB80 80 Shore A (James Walker)




NBR N9002‐90 (Trelleborg)




NBR 70 (Ramsey Services)




NBR70 K6 (GAPI Compounds)




NBR 70 (Eriks Seals)




Nylon 6 (Skiffy)




Nylon XLPE (OEM)




PEEK 450G (Victrex)




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Aging Time


Change %



PEEK 450CA30 (30% Carbon Filled) (Victrex)




PEEK 1000 (OEM)




PEEK W4685 (Parker)




PEEK W4738 (Parker)




Polyamine Imide AMS 3670‐1 (OEM)




Polyamine Imide AMS 3670‐4 (OEM)




Polyurethane (OEM)




POM (Polyoxymethylene) (OEM)




PTFE (OEM)




PTFE (25% Carbon Filled) (OEM)




PTKC (OEM)




PVDF (OEM)




Turon T19 (Trelleborg)




Turcon T29 Step Seal (Trelleborg)




Turcon T40 (Trelleborg)




Turcon T46 (Trelleborg)




Viton 70 (OEM)




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Aging Time


Change %



Viton 90 (OEM)




Viton A 9009‐75 (OEM) 1 week Clear and bright 0.45 0.00



Viton Extreme 90 Shore A

(Clwyd)




Viton HTV90‐A2 90 Shore A (Dupont)




Viton V747‐75

(Parker)




Zurcon Z52 95 Shore A

(Trelleborg)



3 months Clear and bright ‐0.44 5.42

Elastomer Compatibility with CLEO at 250 °C

The results for PTFE & PEEK aged at 250 °C for 3 months are tabulated below.

PEEK 450G (Victrex)




PTFE (OEM)




PTFE and PEEK both meet the requirements of ISO 13628‐6 after aging for 3 months at 250 °C.

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4.9 – Fluid Lubricity and Wear


Both of the following tests have been applied using an independent test laboratory:

1. Shell 4 Ball test (IP 239).

PROCEDURE

1. Shell 4 Ball test (IP 239). The details of the test procedure are given in the IP239. The test

is twofold:

Weld point test – gives an indication of load carrying capability. The steel ball is

loaded and rotated against 3 fixed steel balls for 10 seconds. A rotation speed of

1460 is used. At the end of each 10‐second run, a further weight is loaded onto the

balls and the test re‐run using fresh fluid. The test stops when the balls weld

together. The weld point is the load at which this occurs.

1 hour wear test – gives an indication of the prevention of metal wear. The load and

speed of rotation is fixed to 30kg and 1460 rpm at the start of the test. Fresh fluid is

added and the test is run for 1 hour. After the test, the scars on the 3 fixed balls are

measured and an average taken. This is the Mean Wear Scar Diameter (MWSD).

RESULTS

This testing was conducted independently.

Results obtained for CLEO exceed the requirements in ISO 13628‐6 in all aspects.

4.9.1 – 4 Ball Weld Point Load

The results on the initial weld point tests are given in Table 1 of this report, which shows the weld

point load determined for the two fluids supplied. All tests were started at an initial test load of

40kg and ended at the weld load was achieved. A 10 second load step duration was used for

these tests. The weld point achieved was higher than the minimum 120 kg acceptance criteria

advised by Offshore Environmental Oils.

Table 1 – Results of the Weld Load and Initial Seizure Load tests on CLEO.

Lubricant Initial Test Load

(kg)

Initial Seizure

Load* (kg)

Weld Point Load

(kg)

Duration of

Load steps

(sec)

RPM Comments

CLEO 10 80 >250 10 1470 Wear scars asymmetric

Criteria provided >120

* measured from friction traces

This test showed CLEO passed the specification requiring a weld load of >120 kg.

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4.9.2 – One Hour 4 Ball Wear Test

The results obtained for the one‐hour wear tests at 30 kg load at 1475 (+/‐25) rpm are shown

below in table 2 with the mean wear scar diameters measured for CLEO demonstrating 50% less

wear than the acceptance criteria of 1.2 mm.

Table 2 – Results of the 1 hour wear tests at 30 kg load and 1460 rpm on CLEO.

Lubricant

Scar

Diameter

Rubbing

Direction

Ball 1 (mm)

Scar

Diameter

Right Angle

Direction

Ball 1 (mm)

Scar

Diameter

Rubbing

Direction

Ball 2 (mm)

Scar

Diameter

Right Angle

Direction

Ball 2 (mm)

Scar

Diameter

Rubbing

Direction

Ball 3 (mm)

Scar

Diameter

Right Angle

Direction

Ball 3 (mm)

Average Scar

Diameter

MWSD (mm)

Comments

CLEO 0.72 0.48 0.70 0.48 0.72 0.50 0.600 Wear scars asymmetric

4.10 – Filterability


300 ml (18.3 in3) of control fluid is filtered under specified conditions through a 0.8 µm filter

membrane at a controlled pressure drop of 0.05 MPa (7.25 psi). Filterability is calculated from the

ratio of filtration near the start of filtration, to the filtration rate at specified higher filtered

volume.

PROCEDURE

Reference is made to ISO 13357‐2[43]. The test results should be reported based on “Stage II” only.

The test membranes specified in the standard might not be compatible with water/glycol‐based

control fluids, in which case suitable membranes have to be located. The specified filtration rating

(0.8 µm) shall apply.

For synthetic based oils, the same procedure but with dry and wet oil (0.5% ± 0.05% artificial

seawater added and vigorously mixed in – ultrasound for 1 hour. The sample shall be left for > 10

hours at room temperature, shaken well and then ran through the test). The test membranes

specified in the standard might not be compatible with synthetic oil based control fluids, in which

case suitable membranes have to be located. The filtration rating for this test shall be 1.2 µm.

RESULTS

The result is the ratio between the flow rate at the start of filtration and the flow rate between

200 ml (12.2 in3) and 300 ml (18.3 in3) of filtered volume, and expressed as a percentage.

ACCEPTANCE CRITERIA

The required stage II filterability is 80% or above.

For wet oil: Required stage II filterability requirement is 20% or above.

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RESULTS

The results for CLEO are tabulated below, and show that both the dry and wet oil exceed the

requirements required in ISO 13628‐6. Indeed, both the wet and dry oil give filterability results >

80%.

Fluid Test 1 Test 2 Test 3 Average

Filterability ISO 13628‐6

CLEO (dry) 90.5% 89.2% 86.3% 88.7% Pass

CLEO (wet) +0.5% Sea Water

89.0% 84.2% 85.8% 86.3% Pass

4.11 – Bacterial & Fungal Resistance with Seawater


Bacterial and Fungal resistance is tested by mixing CLEO with synthetic seawater at a ratio of

50:50.

The mixtures will then be aged at temperatures of ambient and / or 40 °C. The level of microbial

infection is monitored on a weekly basis up to 12 weeks and on a monthly basis thereafter. Two

sets of mixtures have been aged as follows:‐

(1) Control fluid with contaminated sea water – ambient and 40 °C.

(2) Control fluid with uncontaminated sea water – ambient and 40 °C.

PROCEDURE

The level of infection is ascertained by immersing a BTM2 dip slide into the test fluid and

incubating the dip slide and comparing the growth with the charts (see overleaf).

The microbes that are highlighted using these dip slides will be bacteria, yeasts and fungus

(moulds). The bacteria form colonies on the colourless agar and the yeasts and moulds form

colonies on the brown agar.

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RESULTS

4.11.1 – CLEO with Contaminated Sea Water at 20 & 40 °C

Aging time CLEO – Ambient CLEO – 40 °C

0 None None

1 week None None

2 weeks None None

3 weeks None None

4 weeks None None

5 weeks None None

6 weeks None None

7 weeks None None

8 weeks None None

9 weeks None None

10 weeks None None

11 weeks None None

12 weeks None None

4 months None None

5 months None None

6 months None None

7 months None None

8 months None None

9 months None None

10 months None None

11 months None None

12 months None None

No bacterial or contamination has been found to date when mixing CLEO with contaminated sea

water. Extensive mould is formed in the sea water sample aged in the absence of any production

control fluids. This suggests that CLEO does not support or promote the growth of bacteria or

fungi in the presence of sea water. Longer term tests are currently on going.

The appearance of both the aged mixtures and the microbial plates are shown overleaf.

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CLEO with contaminated sea water – 20 & 40 °C

CLEO – aged at 20 °C for 12 months


Sea Water Alone (12 weeks).

Fluid Appearance

Both phases clear and bright


Bacteria

Mould

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4.11.2 – CLEO with Uncontaminated Sea Water at 20 & 40 °C

Aging time / Weeks CLEO – Ambient CLEO – 40 °C

0 None None

1 week None None

2 weeks None None

3 weeks None None

4 weeks None None

5 weeks None None

6 weeks None None

7 weeks None None

8 weeks None None

9 weeks None None

10 weeks None None

11 weeks None None

12 weeks None None

4 months None None

5 months None None

6 months None None

7 months None None

8 months None None

9 months None None

10 months None None

11 months None None

12 months None None

No bacterial or contamination has been found to date when mixing CLEO with contaminated sea

water. Extensive mould is formed in the sea water sample aged in the absence of any production

control fluids. This suggests that CLEO does not support or promote the growth of bacteria or

fungi in the presence of sea water. Longer term tests are currently on going.

The appearance of both the aged mixtures and the microbial plates are shown overleaf.

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CLEO with uncontaminated seawater ‐ 20 & 40 °C



Sea Water Alone for 12 weeks

Fluid Appearance



Bacteria

Mould

CLEO ISO 13628-6 Manual Issue 2

Documents

Transcript of CLEO ISO 13628-6 Manual Issue 2