FINAL REPORT: LARGE SCALE ACCELERATED CUI TEST OF E-2000 AND E-1100EG

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1 FINAL REPORT: LARGE SCALE ACCELERATED CUI TEST OF E-2000 AND E-1100EG Prepared for: Elisha Technologies Company L.L.C. P.O. Box 280 Moberly, Missouri Prepared by: Dr. Russell D. Kane InterCorr International, Inc. (formerly CLI International, Inc.) Houston, Texas USA Date: May 14, 1998 Project No: L983475K

2 INTRODUCTION Presented herein are the results of the large scale accelerated corrosion under insulation (CUI) test conducted by InterCorr International, Inc. (formerly CLI International, Inc.) for Elisha Technologies Company L.L.C (Elisha). These tests involved the exposure of two pipe sections and the proposed ASTM CUI test cell to evaluate the effectiveness of two Elisha products surface treatments (E-1100 EG and E-2000) and the new surfaces formed by the Elisha products. This laboratory work was performed over the period January through March, SUMMARY A long term (>900 hour) accelerated CUI test involving variable temperature and wet/dry cycles was conducted on treated and non-treated carbon steel pipe sections. The test conditions and the relative performance of two surface treatments were monitored using the proposed ASTM G CUI test cell with both gravimetric and linear polarization measurements at severely defected areas in the coating. Post test visual examination was also conducted on relatively large treated and non-treated areas on bead blasted and heavily corroded surfaces. The electrochemical and gravimetric evaluations were conducted on both products (E-2000 and E-1100 EG) at intentionally defected areas. Earlier work indicated that no electrochemical corrosion currents were detected under a complete coverage of Elisha products and that the only opportunity for corrosion currents was act locations of severe flaws in the coating. Surface analyses conducted by Elisha has shown that this behavior was produced by surfaces changes (i.e. mineralization) resulting from contact of the metal surface with the Elisha products. The electrochemical measurements showed that Elisha E-2000 and E-1100 EG were to be stable and exhibited high protection efficiency versus bare steel under the same conditions. In addition, E-2000 was applied to relatively large sections of both, bead blasted and heavily corroded surfaces then exposed to the same accelerated test conditions used for the electrochemical tests. Visual examination of E-2000 showed little change or deterioration during the test duration. TECHNICAL APPROACH This laboratory evaluation was conducted to demonstrate the performance of Elisha surface treatment E-2000 under accelerated and severe CUI conditions for an extended period of exposure. The test conditions included cyclic temperature and multiple wet/dry periods. E was applied to two large pipe sections. Following completion of the exposure, the coated and non-coated surfaces were examined in two large areas having different initial pipe surface conditions: (1) a pre-rusted surface and (2) bare steel (glass bead blasted). The test corrosivity versus time was also monitored gravimetrically and electrochemically using the proposed ASTM CUI test cell. Three sets of test electrodes were used in this cell to monitoring three

3 surface conditions: (1) bare steel, (2) E-2000 treated and (3) E-1100 EG treated. Corrosion rates were obtained for both bare and treated materials using gravimetric and electrochemical methods. EXPERIMENTAL PROCEDURE TEST SET-UP Figure 1 shows the test apparatus used to perform the CUI tests. It involves two test sections of nominal 2-inch O.D. pipe used for the large-scale evaluation. Each pipe section had approximately one foot lengths of (1) abrasive cleaning followed by P.7122 epoxy coating, (2) Elisha E-2000 (on a bead blasted surface) and (3) bare steel. An inert tape separated each region on the O.D. surface of the pipe. To simulate the conditions for CUI, the pipe sections were internally heated using an immersion heater and heat transfer oil which conducted the heat to the pipe surface. The temperature of the pipe O.D. surface was controlled using a thermocouple on the O.D. surface and a controller. The pipe was surrounded externally with inert Perlite insulation formed to an I.D. that was about 0.5 inch larger than the pipe O.D. The accelerated CUI test solution was added from a reservoir to the annular space between the pipe and the insulation using a micrometering pump. Cotton gauze was placed around the test sections of the pipe specimens to more uniformly wick the test solution. The proposed ASTM G CUI standard test cell was placed between the two pipe sections. The basic design of the cell is shown in Figure 2. A more detailed description is given in a previous reference. [1] The CUI test cell was used to monitor corrosivity of the CUI conditions on carbon steel and to obtain an indication of relative performance of the two Elisha coatings (E-2000 and E-1100 EG). The evaluation portion of the CUI-Cell consisted of three sets of three rings (one for each material condition) which were electrically isolated using TFE spacers. Intentional defects were placed on the exposed surfaces of the coatings in the coated specimens to concentrate the corrosive attack and to evaluate the response of the coating materials to severe service induced damage. Cotton string was placed in the intentionally defected areas of the coated coupons and around the bare steel coupons to wick the test solution on to the surface. Each set of three rings was a three-electrode linear polarization resistance (LPR) circuit (working electrode, reference electrode and counter electrode) per ASTM G59. They were used to make measurements of instantaneous corrosion rate versus time under CUI conditions for each material condition. In addition to electrochemical measurements, the working electrodes for each material condition were used to determine mass loss corrosion rates using gravimetric measurements per ASTM G31. These corrosion rates were based on actual exposed area determined after exposure and cleaning of the coupons.

4 MATERIALS AND SPECIMENS Pipe material. The CUI tests were conducted on a typical carbon steel pipe material (ASTM A106 Grade B) that was obtained in a 2-inch nominal pipe size. Two, three foot long pipe sections were fitted with slip-on bolted flanges and used to expose a relatively large area of material to CUI conditions. The same material was used for machining the ring coupons in the CUI-Cell. Elisha products. Elisha products have been developed to mineralize the metal surface under the coating. Mineralization is the ability to grow a very thin mineral on metal surfaces for useful purposes, including protection against corrosion. Elisha Engineered Surfaces TM are formed when mineral-forming compounds are delivered to the surface of a metal via novel products, (such as E-2000 and E-1100 EG). The substrate contribute donor ions to react and/or interact with delivered compounds, forming a very thin layer of mineral that is chemically bonded to the surface of the substrate and measured to be only a few monolayers thick [2]. Patent [3] and patent applications cover the delivery of novel formulations was well as the mineralized layer that is formed as a result of the interactions between the applied coating and the underlying substrate. The presence and uniqueness of the mineralized layer has been confirmed by conventional analytical surface methods such as X-ray photoelectron spectroscopy (XPS). TEST ENVIRONMENT The CUI test solution was chosen to accelerate corrosive attack and most likely represent conditions that would be more severe than characteristically found in service. The test solution consisted of 1000 ppm solution of NaCl in distilled water acidified to ph 6.0 with sulfuric acid (H 2 SO 4 ). This solution was pumped into the annular space between the insulation and the pipe O.D. The test temperature was 150 F as measured on the O.D. surface of the pipe. Periodically, the pumping of solution was stopped and the temperature elevated to 230 F and the pipe and CUI-Cell allowed to dry. The point of dry conditions was assessed using the LPR capabilities of the CUI-Cell. Dry conditions were considered to occur at the point were the corrosion rate of the bare steel coupons gave an instantaneous corrosion rate of zero during the drying cycle. RESULTS AND DISCUSSION CUI TEST CELL DATA LPR Data. Figure 3 shows the LPR corrosion rate data versus time for the total test duration, which was just short of 1000 hours. Three curves are indicated: (1) bare steel, (2) E-2000 surface treatment and (3) E-1100 EG surface treatment.

5 The corrosion rate of bare steel in the CUI tests ranged from approximately 5 mpy to 28 mpy for the wet cycle with transient corrosion rates during wet/dry cycling ranging from 0 to about 55 mpy. The trend in the data with time was such that the rate of corrosion rate increased with each wet/dry cycle indicating the increased corrosivity as the exposure progressed. This was most likely due to the concentration of chloride as a result of the multiple wet/dry cycles. By comparison, the corrosion rates for the coupons treated with E-1100 EG and E-2000 were significantly less than that of the bare steel. The corrosion rates for the two treatments during the wet cycle were between 0.25 to about 5.0 mpy with transient corrosion rates of 0 to 7.5 mpy during the drying cycle. These corrosion rates should be considered as worst case values due to the presence of intentional defects in the coatings and the severity of the test solution. The corrosion rates for the E-2000 formulation were slightly less than those obtained for the E EG formulation. Based on the LPR corrosion rates the protection efficiency of the two coatings near the completion of the test were 82 percent (E-1100 EG) and 89 percent (E-2000). Mass Loss Corrosion Data. The mass loss corrosion rates for the same three material conditions obtained from the CUI-Test Cell working electrodes were as shown below: Material Condition Corrosion Rate (mpy) Protection Efficiency Bare Steel E % E-1100 EG % The average mass loss corrosion rate for the bare steel coupon over the exposure period was 20.9 mpy. This was in good agreement with the LPR corrosion rates taking into account the natural change in corrosivity of the CUI conditions with exposure time. Corrosion rates for the two surface treatments were 4.5 mpy and 2.9 which were significantly lower than that for the bare steel coupons and comparable to the corrosion rates determined by LPR measurements. Consequently, the protection efficiencies for the coatings shown above were also similar to those determined from the LPR data. As in the case of the LPR data, the corrosion rates presented should be considered worst case values due to the presence of intentional coating defects and the severity of the test solution. Visual examination of the coupons indicated that corrosion was essentially limited to the regions were the coatings were removed that contained the wicks. Areas of intact coating on the coupons showed no signs of corrosion. EXAMINATION OF THE PIPE SECTIONS Following approximately 950 hours of CUI exposure the pipe samples were removed from test and examined for deterioration. A detailed photographic record was made of the tests on the pipe sections and the performance of the Elisha coatings (E-2000 and E-1100 EG). This is given in Appendix I through III. Based on the visual examination, the following observations were made:

6 1. The layer produced on the O.D. surface of the pipe by the E-2000 treatment did not change or deteriorate; however, with one exception (See Item 2 below). 2. On the bottom of the pipe section cleaned by bead blasting, a portion of the E-2000 material disbonded and had broken loose from the pipe. It was found laying in the bottom of the insulation. This occurred in the same area where a liquid/vapor interface had occurred during the test. It appeared that during the drying cycle at 230 F, the water boiled and disbonded the coating from the relatively smooth surface of the bead blasted metal. Subsequent tests conducted in boiling water showed this same effect on smooth bead blasted specimens. However, specimens given a rougher surface by abrasive blasting showed no disbonding of the coatings under the same conditions. 3. In the abovementioned region on the bead blasted pipe, where the coating was disbonded and separated from the pipe, some rusting occurred. Some of the rust appeared to be from the resultant unprotected (non-treated) end of the same pipe and some from the disbonded region. 4. The pipe surface tested with the intentionally pre-rusted condition showed no evidence of disbonding of the E-2000 coating at the bottom of the pipe. The coatings had excellent adhesion to the rusted metal surface, which had been conditioned only by wire brushing prior to the E-2000 treatment. 5. The P.7122 epoxy coated coupons placed between the pipe and insulation in each test section of the CUI apparatus were scribed prior to exposure on both top and bottom surfaces. In the test section with the disbonded layer (See Item 2 above), the top of the coupon contacting the disbonded material showed no rusting of the metal in the scribe. The opposite surface of the coupon, showed light rusting of the metal in the scribed region. 6. In the pre-rusted region of the pipe, a second coupon was placed in the bottom of the insulation in contact with the treated pipe. The side of the coupon in contact with the E treated area showed no evidence of rusting in the scribe. The opposite surface of the coupon showed light rusting in the scribe. 7. The portion of the pipe that was abrasive blasted and coated with a P.7122 epoxy coating was in good condition. However, the coating was starting to disbond and peel along the edge of the coating adjacent to a scribe mark placed in the coating prior to testing and rusting was observed on the metal in the scribe mark. 8. Removal of the E-2000 layer on the bead blasted pipe at locations in the middle and ends of the treated section revealed complete protection. No localized corrosion or under coating attack was noted in the region covered with the E-2000 layer.

7 9. Removal of the E-2000 layer on the pre-rusted surface also showed no change in appearance of the pre-rusted surface when compared to the original rusted surface. CONCLUSIONS Based on the results presented herein the following conclusions were made: 1. Laboratory simulation of accelerated CUI conditions produced steady state corrosion rates on bare steel surfaces that were up to about 30 mpy with up to 55 mpy during wet/dry transients. 2. Corrosion rates for bare steel increased with each wet/dry cycle. 3. Both E-2000 and E-1100 EG treatments resulted in a significant reduction in the corrosive attack under accelerated CUI conditions. Worst case steady state corrosion rates in the defected areas on coated specimens were less than 5 mpy. Based on a nominal 0.1 inch corrosion allowance this would result in an expected surface life of 20 years versus about 3 years for the untreated bare steel. 4. Protection efficiencies for these coating materials were between 82 and 89 percent using LPR data and 78 to 86 percent based on mass loss corrosion data. 5. The E-2000 coating showed good performance over large areas (both bead blasted and prerusted) with no significant changes in appearance over the test period, except for one case. This was the location on the bead blasted region on the pipe at the liquid/vapor interface where local boiling occurred. However, steel with a rougher surface finish (as produced by abrasive blasting) was found not to exhibit this behavior. 6. Coupons coated with P.7122 epoxy coating were found to be protected when in contact with the E-2000 material. 7. The sections of the test pipe coated with P.7122 epoxy coating intentionally damaged with a scribe mark showed evidence of corrosion in the scribe mark and disbonding of the coating adjacent to the scribe. It was a pleasure working with you and to be of continued support to Elisha Technologies development efforts. If you have any questions or need further assistance, please contact the undersigned. Sincerely,

8 Dr. Russell D. Kane President Dr. Michael S. Cayard Vice President RDK-C-MD/Reports/983475K-ElishaCUI

9 REFERENCES 1. D. Abayarathna, W.G. Ashbaugh, R.D. Kane, N.G McGowen and R.L. Heimann, Measurement of Corrosion Under Insulation and Effectiveness of Protective Coatings, Corrosion/97, Paper No. 266, NACE International, Houston, Texas March J.J. Hahn, N.G. McGowen and R.L. Heimann, Modification and Characterization of Mineralization Surface for Corrosion Protection, Surface and Coatings Technology, Submitted for Publication, Heimann, R. H. Corrosion Resistant Buffers for Metal Systems. U.S. Patent 5,714,093, 1998

10 Figure 1 - Schematic of large scale CUI test apparatus.

11 Figure 2 - Detailed schematic of proposed ASTM G CUI-Test Cell.

12 Figure 3 - LPR corrosion rate versus time for three conditions (bare steel, E-2000 and E-1100 EG) in CUI-Test Cell. Electrochemical measurements were made at areas where the coating was intentionally removed to simulate severe physical damage.

13 APPENDIX I - PHOTOGRAPHIC RECORD OF PIPE SECTION TEST FOR (E-2000 AND E-1100 EG)

14 APPENDIX II - PHOTOGRAPHS OF MID-TEST EXAMINATION

15 APPENDIX III - PHOTOGRAPHS OF POST TEST EXAMINATION

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