R Ballast tank coating testing of Jotacote F60 on Muki Z ... NORSKE VERITAS TM REPORT Ballast tank coating testing of Jotacote F60 on Muki Z 2001 shop primer Jotun AS Report No./DNV

DET NORSKE VERITASTM

REPORT

Ballast tank coating testing of Jotacote

F60 on Muki Z 2001 shop primer

Jotun AS

Report No./DNV Reg No.: 2012-5029 / 13FNOZF-5

Rev 00, 2012-08-17

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Ballast tank coating testing of Jotacote F60 on Muki Z 2001 shop primer

DNV Reg. No.: 13FNOZF-5 Rev. No.: 00 Date : 2012-08-17 Page ii of ii

Table of Contents

1 INTRODUCTION ............................................................................................................. 1

2 SCOPE OF WORK ........................................................................................................... 1

3 WORK CARRIED OUT PRIOR TO EXPOSURE ....................................................... 1

3.1 Primary surface preparation ....................................................................................... 1

3.2 Application ................................................................................................................. 2

3.2.1 Application procedure ......................................................................................... 2 3.2.2 Panel coding ........................................................................................................ 4 3.2.3 Dry film thickness................................................................................................ 5

3.3 Pinhole detection ........................................................................................................ 7

4 EXPOSURE ........................................................................................................................ 7

5 PRODUCT IDENTIFICATION ...................................................................................... 7

6 EXAMINATIONS AND TESTS CARRIED OUT AFTER EXPOSURE .................... 7

7 EVALUATION OF TEST RESULTS ............................................................................. 8

8 CONCLUSION .................................................................................................................. 8

9 REFERENCES .................................................................................................................. 9

Appendix A Weathering data Appendix B Infrared spectra Appendix C Detailed test results Appendix D Photo documentation

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DNV Reg. No.: 13FNOZF-5 Rev. No.: 00 Date : 2012-08-17

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1 INTRODUCTION The coating system, JOTACOTE F60 applied to steel panels shop primed with MUKI Z 2001, has been tested in accordance with the IMO Performance Standard for Protective Coatings /1/.

2 SCOPE OF WORK The following work and tests have been performed by JOTUN A/S at the JOTUN A/S test laboratory in Sandefjord, Norway, partly under supervision of a representative from DNV:

- Surface preparations as described in Table 1 and 2 - Application processes as documented in Table 3 - Two months outdoor weathering of the shop primed test panels The following work and tests have been performed by DNV at the DNV laboratory in Bergen, Norway: - Identification of the coating system by means of determination of density and infrared (IR)

spectra - Total dry film thickness measurements and pinhole detection on the test panels before testing - 180 days exposure in an exposure tank with wave movement (see Figure 1 for details) - 180 days in dry heat (see Figure 1 for details) - 180 days in condensation chamber (see Figure 1 for details) - Evaluation of testing performed after exposure, including visual check for rust and blisters,

undercutting from scribe, adhesion measurements and coating flexibility - Evaluation of cathodic protection during wave tank exposure

3 WORK CARRIED OUT PRIOR TO EXPOSURE

3.1 Primary surface preparation

The primary surface preparation was carried out as described in Table 1.

Table 1 Primary surface preparation data*

Surface preparation date 2011.05.19

Surface preparation method Gritblasted with Alsil. A3 .

Blasting standard Sa 2½

Roughness Medium

Water soluble salts Average: 17 mg/m2

Dust and abrasive inclusions No dust or abrasive contaminations were observed on the surface

* Data provided by Jotun AS

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3.2 Application

3.2.1 Application procedure

MUKI Z 2001 was applied to the test panels according to the application data given in Table 3.

The shop primed test panels were weathered outdoors for two months. Details on the weathering process and the following cleaning of the test panels are provided in Table 2, while further meteorological data of the weathering period are attached as Appendix A.

Table 2 Secondary surface preparation and weathering details*

Weathering site (outdoor) At the JOTUN AS site in Sandefjord, Norway

Start of weathering 2011-06-21: W3, W4 2011-06-29: W1, W2, H, C2 2011-07-07: C1

Stop of weathering 2011-09-08: all panels

Preparation of test panel after the weathering period

Cleaned with low pressure washing

* Data provided by Jotun AS

Two coats of JOTACOTE F60 were applied to the weathered and cleaned shop primed test panels. The complete application data are given in Table 3.

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Table 3 Application data

Coating data Shop primer Shop primer 1st coat 2nd coat

Paint system MUKI Z 2001 MUKI Z 2001 JOTACOTE F60 JOTACOTE F60

Grey Grey Grey White

Panels (DNV code) W3, W4 W1, W2, H, C1, C2 All All

Manufacturer Jotun AS

Date 2011.05.26 2011.06.09 2011-09-20 2011-09-21

Time 11:10 11:15 10:55 11:00

Batch no. paste/base Comp. B / paste: FR0111226670

Comp. B / paste: FR0111226670

Lab made Lab made

Batch no. liquid/hardener Comp. A / liquid: FR4110288151

Comp. A / liquid: FR4110288151

Lab made Lab made

Thinner name (if used) Not used Not used Not used Not used

Batch no. thinner NA NA NA NA

Equipment used (pressure ratio)

WIWA (60:1) WIWA (60:1) WIWA (60:1) WIWA (60:1)

Air pressure at nozzle [bar]

150 150 150 150

Size nozzle [inch] 0.015 0.015 0.019 0.019

Fan width [º] 40 40 40 40

Mix. ratio by weight A : B = 40 : 60

A : B = 40 : 60

A : B = 100 : 15

A : B = 100 : 15

Induction time [min] - - 10 10

Volume solids [%] 28 28 60 60

Wet film thickness [µm] 70 70 270 270

Dry film thickness [µm] 20 20 160 See Table 4

Thinner [volume%] 0 0 0 0

Air temperature [ºC] 15 19 17 16

Humidity [% RH] 72 78 68 58

Steel temp. [ºC] 13 19 18 18

Dew point [ºC] 10 15 11 7

Comments: Present during the application of shop primer: Reidar J. Pettersen, Terje Aamodt and Odd Arntzen – Jotun A/S Monika Næss – Det Norske Veritas Present during the application of 1st and 2nd coat: Reidar J. Pettersen, Puc van Hoang, Odd Arntzen and Ingvild Guro Sageng – Jotun A/S. Monika Næss – Det Norske Veritas. Touch-up was done on both u-beams (W3 and W4 panels) due to damage during freight. Date of toch-up was 21st of December 2011, done by DNV Bergen, using the grey Jotacote F60.

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3.2.2 Panel coding

The panels were coded with the unique DNV system name J34Z followed by a suffix specific for every panel’s position during the six-month exposure testing as shown in Figure 1.

Figure 1 Panel coding

H

W1 top

C1 C2 R1

W4 side (not cooled)

W3 side (cooled)

W2 bottom

Wave tank (size: 400x200 mm)

Condensation chamber (size: 150x150 mm)

Heating cabinet (size: 400x200 mm)

anode

artificial holiday

scribe scribe

U-beam U-beam

scribe

Reference (size: 150x150 mm)

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3.2.3 Dry film thickness The dry film thickness (DFT) measurements of the total coat were carried out by means of a calibrated Elcometer 456 using the template shown in Figure 2. Table 4 shows the results from the measurements of the total dry film thickness.

Panel coding on the reverse side

21 3

54 6

87 9

1110 12

1413 15

Panel coding on the reverse side

1 2 3

7 8 9

4 5 6

Figure 2 DFT measurements locations

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Table 4 Results from the DFT measurements of the total coat, values are given in m (20 m subtracted for shop primer)

Measuring point

(according to Figure 2)

Panel

W1 W2 W3 W4 H C1 C2 Total

1 356 402 390 400 322 354 382

2 394 418 418 410 366 362 382

3 356 390 360 366 320 366 376

4 346 332 356 388 348 372 418

5 398 350 396 438 354 412 416

6 380 354 366 364 322 402 394

7 350 352 344 368 330 406 362

8 366 386 376 398 338 396 362

9 370 354 322 338 316 366 346

10 350 362 354 374 358

11 404 354 406 416 392

12 392 348 360 354 344

13 396 346 336 350 370

14 456 414 394 382 412

15 432 390 356 322 338

Max 456 418 418 438 412 412 418 456

Min 346 332 322 322 316 354 346 316

Average 383 370 369 378 349 382 382 372

StDev 32 27 27 31 28 22 24 30

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3.3 Pinhole detection

Pinhole detection was performed on the coated test panel before the tank exposure. The detection was carried out by means of an Elcometer 269 Pinhole detector at 90 volts. The results from the pinhole detection are presented in Table 6.

4 EXPOSURE The exposure in the simulated ballast wave tank, condensation chamber and heating cabinet was carried out according to the IMO Performance Standard for Protective Coatings /1/. The exposure was started 2012-01-18 and terminated 2012-07-16.

5 PRODUCT IDENTIFICATION

The density of each component of the coating system was determined by means of a TQC Mod. VF20971 pycnometer based on ISO 2811-1 /5/. Furthermore, IR spectra of all components were recorded on a Nicolet Protégé 460 FT-IR spectrometer. The results from the paint identification are listed in Table 5 and Appendix B respectively.

Table 5 Product identification analysis

Product Batch no. Density [g/ml] Infrared identification

MUKI Z 2001 (Paste / Comp B)

FR0111226670 2.05 See Appendix B, Figure B1

MUKI Z 2001 * (Liquid / Comp A)

FR0211230211 0.91 See Appendix B, Figure B2

JOTACOTE F60, Grey (Base / Comp A)

Lab made 1.48 See Appendix B, Figure B3

JOTACOTE F60, White ** (Base / Comp A)

Lab made 31.01.12

1.51 See Appendix B, Figure B4

JOTACOTE F60, (Hardener / Comp B)

Lab made 0.92 See Appendix B, Figure B5

* Samples from the batch used for application were dry upon arrival and could not be analysed. However, sample from Muki Z 2001 component A was analysed by DNV in 2011. ** This sample was provided by Jotun A/S in april 2012, and analysed by DNV.

6 EXAMINATIONS AND TESTS CARRIED OUT AFTER EXPOSURE

The visual inspection for blisters and rust as well as the adhesion testing were carried out according to specifications and standards referred to in the IMO Performance Standard for Protective Coatings /1/. In addition, the evaluation of cathodic protection was performed in accordance with ISO 15711:2003 /5/, ASTM G8:1996 /6/ and further IACS Rec. No. 101 /7/. Interpretation details are given in the present report. The results of the examinations are schematically given in Table 6 and more detailed in Appendix C. Pictures of the panels after exposure as well as pictures of the adhesion tests are enclosed as Appendix D.

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7 EVALUATION OF TEST RESULTS

The test results have been evaluated in accordance with the requirements for epoxy-based systems on shop primed and two-month weathered steel substrate stated in the Performance Standard for Protective Coatings /1/. The results from this evaluation are presented in Table 6.

Table 6 Results from evaluation of the coated test samples

Test parameter Acceptance criteria /1/ Test results Evaluation

Blisters on panel 1) No blisters No blisters Passed

Rust on panel 1) No rust No rust Passed

Number of pinholes 2) 0 0 Passed

Adhesion values – average wave tank panels [MPa] 3)

> 3.5 adhesive failure

≥ 3 cohesive failure

8.5 Passed Total adhesive: 0 %

Total cohesive: 100 %

Adhesion values –average condensation chamber panels [MPa] 4)

> 3.5 adhesive failure

≥ 3 cohesive failure

7.6 Passed Total adhesive: 0 %

Total cohesive: 100 % Current demand – wave tank bottom panel [mA/m2] 5)

< 5 1.3 Passed

Cathodic disbondment – wave tank bottom panel [mm] 5)

< 8 0 - 1 Passed

Undercutting from scribes – average maxima of wave tank panels [mm] 6)

< 8 1.3 Passed

U-bar / U-beam

Any defects, cracking or detachment at the angle or weld will lead to system being failed.

No defects, cracking or detachment

Passed

1) See Appendix C, Table C1 for details 2) See chapter 3.3 for details 3) See Appendix C, Table C2 for details 4) See Appendix C, Table C3 for details 5) See Appendix C, Table C5 for details 6) See Appendix C, Table C6 for details

8 CONCLUSION The coating system, two coats of JOTACOTE F60 applied to steel panels shop primed with MUKI Z 2001, has been tested in accordance with the IMO Performance Standard for Protective Coatings /1/.

Based on the results and evaluations described in the present report, the coating system JOTACOTE F60 applied to MUKI Z 2001, both products from JOTUN AS, has passed the test requirements for epoxy-based systems given in the IMO Performance Standard for Protective Coatings /1/.

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9 REFERENCES

/1/ IMO MSC.215(82):2006 Performance Standard for Protective Coatings for dedicated sea water ballast tanks in all types of ships and double-side skin spaces of bulk carriers (including all official standards referred to therein).

/2/ ISO 8503-4:1988 Preparation of steel substrates before application of paints and related products - Surface roughness characteristics of blast-cleaned steel substrates - Part 4: Method for the calibration of ISO surface profile comparators and for the determination of surface profile - Stylus instrument procedure.

/3/ ISO 8502-6:2006 Preparation of steel substrates before application of paints and related products – Tests for the assessment of surface cleanliness – Part 6: Extraction of soluble contaminants for analysis - The Bresle method.

ISO 8502-9:1998 Preparation of steel substrates before application of paints and related products – Tests for the assessment of surface cleanliness Part 9: Field method for the conductometric determination of water-soluble salts.

/4/ ISO 2811-1:1997 Paint and varnishes - Determination of density – Part 1: Pycnometer method.

/5/ ISO 15711-2:2002 Paints and varnishes - Determination of resistance to cathodic disbonding of coatings exposed to sea water.

/6/ ASTM G8:1996 Standard test method for cathodic disbonding of pipeline coats

/7/ IACS Rec. No. 101: 2008 Model Report for IMO Resolution MSC.215(82) Annex 1 “Test Procedures for Coating Qualification”.

/8/ ISO 4628-2:2003 Paint and varnishes - Evaluation of degradation of coatings - Designation of quantity and size of defects, and of intensity of uniform changes in appearance - Part 2: Assessment of degree of blistering.

/9/ ISO 4628-3:2003 Paint and varnishes - Evaluation of degradation of coatings - Designation of quantity and size of defects, and of intensity of uniform changes in appearance - Part 3: Assessment of degree of rusting.

/10/ ISO 4628-8:2005, (section 5.3.1) Paints and varnishes - Evaluation of degradation of coatings - Designation of intensity, quantity and size of common types of defects, and of intensity of uniform changes in appearance - Part 8: Assessment of degree of delamination and corrosion around a scribe.

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APPENDIX A

WEATHERING DATA

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The weathering of the shop primed test panels was carried out at the JOTUN AS site in Sandefjord, Norway. The meteorological data was obtained from The Norwegian Meteorological Institute. Melsom is the name of the nearest weather station that records temperature. Melsom is located a few km from Sandefjord.

Figure A1: The weathering conditions during the exposure, July 2011

Figure A2: The weathering conditions during the exposure, August 2011

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APPENDIX B

INFRARED SPECTRA

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OSL1114987_007

Name

16264-11

Description

4000 6503500 3000 2500 2000 1500 1000

106

22

30

40

50

60

70

80

90

100

cm-1

%T

Figure B1 IR spectra of MUKI Z 2001 (binder phase of paste), batch no.: FR0111226670

4000,0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 650,0

-0,040,0

0,1

0,2

0,3

0,4

0,5

0,6

0,7

0,8

0,9

1,0

1,1

1,2

1,3

1,4

1,5

1,6

1,7

1,8

1,9

1,95

cm-1

A

Figure B2 IR spectra of MUKI Z 2001 (liquid), batch no.: FR0211230211

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16264-14

Name Description

4000 6503500 3000 2500 2000 1500 1000

102

35

40

45

50

55

60

65

70

75

80

85

90

95

100

cm-1

%T

Figure B3 IR spectra of JOTACOTE F60 Grey (binder phase of base), batch no.: Lab made

OSL1205653 284-14

Name

Sample 040 By Alin Date fredag, mai 25 2012

Description

4000 6503500 3000 2500 2000 1750 1500 1250 1000 750

105

35

40

45

50

55

60

65

70

75

80

85

90

95

100

cm-1

%T

Figure B4 IR spectra of JOTACOTE F60 White (binder phase of base), batch no.: Lab made 31.01.12

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16264-15

Name Description

4000 6503500 3000 2500 2000 1500 1000

101

48

50

55

60

65

70

75

80

85

90

95

100

cm-1

%T

Figure B5 IR spectra of JOTACOTE F60 (hardener), batch no.: Lab made

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APPENDIX C

DETAILED TEST RESULTS

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Table C1 Development of blisters and rust after exposure

Panel Blisters7) Rust 8) Other defects

W1 0 0 0

W2 0 0 0

W3 0 0 0

W4 0 0 0

H 0 0 0

C1 0 0 0

C2 0 0 0

7) The of the degree of blistering was performed according to ISO 4628-2 /8/ 8) The evaluation of degree of rusting was performed according to ISO 4628-3 /9/

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Table C2 Results of the pull-off adhesion test: wave tank and heat panels

Panel

Adhesion test no.9)

Adhesion strength [MPa] 10) Fracture [%] 11)

W1

1 8.7 1B, 99C

2 8.9 1B, 99C

3 7.9 1B, 99C

W2

4 8.8 2B, 98C

5 7.1 2B, 98C

6 8.4 2B, 98C

W3

7 8.6 1B, 99C

8 9.2 1B, 99C

9 7.9 1B, 98C, 1D

W4

10 9.7 100C

11 9.1 1B, 99C

12 7.5 92C, 8D

H

13 8.5 1B, 98C, 1D

14 9.4 1B, 99C

15 8.4 1B, 99C

Average 8.5 Total adhesive: 0 % Total cohesive: 100 %

Maximum 9.7

Minimum 7.1

9) Number of test specimen per panel in accordance with IACS Rec. No. 101 /7/.

10) Adhesion tests were carried out with a DeFelsko PosiTest AT adhesion tester. Dollies with 20 mm diameter were used. The coating surface and dollies were softly grinded with FEPA P#320 SiC paper and rinsed with technical alcohol. The dollies were glued to the coated surface with 3M DP410 adhesive. The curing of the adhesive was carried out according to manufacturer’s recommendations. A hole saw was employed to carefully cut through the coating down to bare steel before pulling off the dollies.

11) A/B: Fracture between the steel surface and the shop primer

B: Fracture in the shop primer

B/C: Fracture between the shop primer and the first coat

C: Fracture in the first coat

C/D: Fracture between the first coat the second coat

D: Fracture in the second coat

-/Y: Fracture between the second coat and the glue

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Table C3 Results of the pull-off adhesion test: condensation chamber panels

Panel

Adhesion test no.9)


C1

16 7.6 3B, 97C

17 7.6 2B, 98C

18 7.1 3B, 97C

C2

19 7.9 1B, 99C

20 7.5 3B, 97C

21 7.8 1B, 99C

Average 7.6 Total adhesive: 0 % Total cohesive: 100 %

Maximum 7.9

Minimum 7.1

9) Number of test specimen per panel in accordance with IACS Rec. No. 101 /7/.









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Table C4 Results of the pull-off adhesion test: reference panel* (for information only)

Panel

Adhesion test no.9)


R1

22 NA NA

23 NA NA

24 NA NA

25 NA NA

26 NA NA

27 NA NA

Average NA NA

Maximum NA

Minimum NA

* No reference panel provided by the Client. 9) Number of test specimen per panel in accordance with IACS Rec. No. 101 /7/









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Table C5 Cathodic protection

Cathodic disbondment [mm] 12) Zinc anode weight loss [g] Current demand [mA/m2] 13)

0 - 1 0.4766 1.3

12) “Assess loss of adhesion at the artificial holiday by using a sharp knife to make two cuts through the coating to the substrates, intersection at the holiday. With the point of the knife, attempt to lift and peel back the coating from around the holiday. Record whether the adhesion of the coating to the substrate has been reduced and the approximate distance, in millimetres, that the coating can be peeled.” (From ISO 15711:2003 /5/) Additionally IACS interpretation of IMO PSPC: “Repeat the cutting and lifting all around the artificial holiday to find the maximum loss of adhesion. Disbonding from artificial holiday can be either loss of adhesion to the steel substrate or between the shop primer and the epoxy coating and shall be less than 8 mm for epoxy based systems to be acceptable (compatibility test). Cohesive adhesion failure in the shop primer is not to be included as part of the loss of adhesion” (from IACS Rec. No. 101 /7/). 13) Exposure time: 119 days submerged in natural seawater during total 180 days of cyclic exposure as defined in /1/

Utilisation factor: 0.8

Consumption rate for Zn-anodes: 11.3 kg/A year

Table C6 Undercutting from scribes

Panel Undercutting from scribes [mm] 14)

W1 2

W3 0 - 1

W4 1

Average 1.3

14) “Rinse the test panel with fresh water immediately after exposure, […], and inspect for visible changes. Carefully remove any loose coating using a knife blade held at an angle, positioning the blade at the coating/ substrate interface and lifting the coating away from the substrate.” (From ISO 4628-8:2005, section 5.3.1 /10/) Additionally IACS interpretation: Undercutting from scribe can be either corrosion of the steel substrate or delamination between the shop primer and the epoxy coating (compatibility test). For PSPC maximum width is used (MSC.215(82), Appendix 1, section 2.2.6). The average of three maximum records of three panels with scribe is used for acceptance. Cohesive adhesion failure in the shop primer is not to be included as part of the delamination. (From IACS Rec. No. 101 /7/)

Table C7 Flexibility (for information only)

Panel Diameter of Mandrel [mm] 15) Elongation [%] 16) Comments

R * NA NA NA

W1 300 1 Several tiny cracks

* No reference panel provided by the Client. 15) Maximum diameter of mandrel for which any cracking in the coating occurs

16) Calculated respectively to the diameter of the mandrel for which any cracking occurs.

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APPENDIX D

PHOTO DOCUMENTATION

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Figure D1 Overview picture of the wave tank panels after exposure and testing (above from left

to right: C1, C2, and H. Below from left to right: W1, W2, W3 and W4)

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Figure D2 Small cracks in the coating after flexibility test (W1 panel)

Figure D3 Undercut scribe on the top wave tank panel (W1)

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Figure D4 Artificial holiday and cathodic disbondment from the artificial holiday on

the wave tank bottom panel (W2)

Figure D5 Undercut scribe on the side wave tank panel with cooling (W3)

Figure D6 Undercut scribe on the side wave tank panel (W4)

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Figure D7 Adhesion test no. 1, 2 and 3 (left to right)


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R Ballast tank coating testing of Jotacote F60 on Muki Z ... NORSKE VERITAS TM REPORT Ballast tank coating testing of Jotacote F60 on Muki Z 2001 shop primer Jotun AS Report No./DNV