DET NORSKE VERITAS TM

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1 TM REPORT Ballast tank coating testing of Jotacote F60 on Muki Z 2001 shop primer Jotun AS Report No./DNV Reg No.: / 13FNOZF-5 Rev 00,

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3 Table of Contents 1 INTRODUCTION SCOPE OF WORK WORK CARRIED OUT PRIOR TO EXPOSURE Primary surface preparation Application Application procedure Panel coding Dry film thickness Pinhole detection EXPOSURE PRODUCT IDENTIFICATION EXAMINATIONS AND TESTS CARRIED OUT AFTER EXPOSURE EVALUATION OF TEST RESULTS CONCLUSION REFERENCES... 9 Appendix A Weathering data Appendix B Infrared spectra Appendix C Detailed test results Appendix D Photo documentation Page ii of ii

4 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 days exposure in an exposure tank with wave movement (see Figure 1 for details) days in dry heat (see Figure 1 for details) 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 Surface preparation method Gritblasted with Alsil. A3. Blasting standard Sa 2½ Roughness Medium Water soluble salts Average: 17 mg/m 2 Dust and abrasive inclusions No dust or abrasive contaminations were observed on the surface * Data provided by Jotun AS Page 1 of 9

5 3.2 Application 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) Start of weathering Stop of weathering Preparation of test panel after the weathering period At the JOTUN AS site in Sandefjord, Norway : W3, W : W1, W2, H, C : C : all panels 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. Page 2 of 9

6 Table 3 Application data Coating data Shop primer Shop primer 1 st coat 2 nd 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 Time 11:10 11:15 10:55 11:00 Batch no. paste/base Comp. B / paste: FR Comp. B / paste: FR Lab made Lab made Batch no. liquid/hardener Comp. A / liquid: FR Comp. A / liquid: FR 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) Air pressure at nozzle [bar] WIWA (60:1) WIWA (60:1) WIWA (60:1) WIWA (60:1) Size nozzle [inch] Fan width [º] Mix. ratio by weight A : B = 40 : 60 A : B = 40 : 60 A : B = 100 : 15 A : B = 100 : 15 Induction time [min] Volume solids [%] Wet film thickness [µm] Dry film thickness [µm] See Table 4 Thinner [volume%] Air temperature [ºC] Humidity [% RH] Steel temp. [ºC] Dew point [ºC] 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 1 st and 2 nd 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 21 st of December 2011, done by DNV Bergen, using the grey Jotacote F60. Page 3 of 9

7 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. Condensation chamber (size: 150x150 mm) Reference (size: 150x150 mm) C1 C2 R1 Wave tank (size: 400x200 mm) W1 top W2 bottom W3 side (cooled) W4 side (not cooled) scribe anode scribe scribe artificial holiday U-beam U-beam H Heating cabinet (size: 400x200 mm) Figure 1 Panel coding Page 4 of 9

8 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 Panel coding on the reverse side Figure 2 DFT measurements locations Page 5 of 9

9 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 Max Min Average StDev Page 6 of 9

10 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 and terminated PRODUCT IDENTIFICATION The density of each component of the coating system was determined by means of a TQC Mod. VF20971 pycnometer based on ISO /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) MUKI Z 2001 * (Liquid / Comp A) JOTACOTE F60, Grey (Base / Comp A) FR See Appendix B, Figure B1 FR See Appendix B, Figure B2 Lab made 1.48 See Appendix B, Figure B3 JOTACOTE F60, White ** (Base / Comp A) Lab made 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 ** 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. Page 7 of 9

11 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 Total adhesive: 0 % Total cohesive: 100 % Passed Adhesion values average > 3.5 adhesive failure 7.6 condensation chamber panels [MPa] 4) Passed 3 cohesive failure Total adhesive: 0 % Total cohesive: 100 % Current demand wave tank bottom panel [ma/m 2 ] 5) < Passed Cathodic disbondment wave tank bottom panel [mm] 5) < Passed Undercutting from scribes average maxima of wave tank panels [mm] 6) < Passed U-bar / U-beam 1) 2) 3) 4) 5) 6) See Appendix C, Table C1 for details See chapter 3.3 for details See Appendix C, Table C2 for details See Appendix C, Table C3 for details See Appendix C, Table C5 for details See Appendix C, Table C6 for details Any defects, cracking or detachment at the angle or weld will lead to system being failed. No defects, cracking or detachment Passed 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/. Page 8 of 9

12 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 :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 :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 :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 :1997 Paint and varnishes - Determination of density Part 1: Pycnometer method. /5/ ISO :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 :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 :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 :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. - o0o - Page 9 of 9

13 APPENDIX A WEATHERING DATA Page A1 of A2

14 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 o0o - Page A2 of A2

15 APPENDIX B INFRARED SPECTRA Page B1 of B4

16 %T Name OSL _007 Description cm-1 Figure B1 IR spectra of MUKI Z 2001 (binder phase of paste), batch no.: FR ,95 1,9 1,8 1,7 1,6 1,5 1,4 1,3 1,2 1,1 1,0 A 0,9 0,8 0,7 0,6 0,5 0,4 0,3 0,2 0,1 0,0-0, , ,0 cm-1 Figure B2 IR spectra of MUKI Z 2001 (liquid), batch no.: FR Page B2 of B4

17 %T Figure B Name Description cm-1 IR spectra of JOTACOTE F60 Grey (binder phase of base), batch no.: Lab made %T Name OSL Description Sample 040 By Alin Date fredag, mai cm-1 Figure B4 IR spectra of JOTACOTE F60 White (binder phase of base), batch no.: Lab made Page B3 of B4

18 %T Figure B5 Name Description cm-1 IR spectra of JOTACOTE F60 (hardener), batch no.: Lab made - o0o - Page B4 of B4

19 APPENDIX C DETAILED TEST RESULTS Page C1 of C6

20 Table C1 Development of blisters and rust after exposure Panel Blisters 7) Rust 8) Other defects W W W W H C C ) The of the degree of blistering was performed according to ISO /8/ 8) The evaluation of degree of rusting was performed according to ISO /9/ Page C2 of C6

21 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) B, 99C W B, 99C B, 99C B, 98C W B, 98C B, 98C B, 99C W B, 99C B, 98C, 1D C W B, 99C C, 8D B, 98C, 1D H B, 99C B, 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 Page C3 of C6

22 Table C3 Results of the pull-off adhesion test: condensation chamber panels Panel Adhesion test no. 9) Adhesion strength [MPa] 10) Fracture [%] 11) B, 97C C B, 98C B, 97C B, 99C C B, 97C B, 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/. 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 Page C4 of C6

23 Table C4 Results of the pull-off adhesion test: reference panel* (for information only) Panel Adhesion test no. 9) Adhesion strength [MPa] 10) Fracture [%] 11) 22 NA NA 23 NA NA R1 24 NA NA 25 NA NA 26 NA NA 27 NA NA Average NA NA Maximum Minimum NA NA * No reference panel provided by the Client. 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 Page C5 of C6

24 Table C5 Cathodic protection Cathodic disbondment [mm] 12) Zinc anode weight loss [g] Current demand [ma/m 2 ] 13) ) 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 ) 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 :2005, section /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 W 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. Page C6 of C6

25 APPENDIX D PHOTO DOCUMENTATION Page D1 of D8

26 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) Page D2 of D8

27 Figure D2 Small cracks in the coating after flexibility test (W1 panel) Figure D3 Undercut scribe on the top wave tank panel (W1) Page D3 of D8

28 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) Page D4 of D8

29 Figure D7 Adhesion test no. 1, 2 and 3 (left to right) Figure D8 Adhesion test no. 4, 5 and 6 (left to right) Page D5 of D8

30 Figure D9 Adhesion test no. 7, 8 and 9 (left to right) Figure D10 Adhesion test no. 10, 11 and 12 (left to right) Page D6 of D8

31 Figure D11 Adhesion test no. 13, 14 and 15 (left to right) Figure D12 Adhesion test no. 16, 17 and 18 (left to right) Page D7 of D8

32 Figure D13 Adhesion test no. 19, 20 and 21 (left to right) - o0o - Page D8 of D8

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