Evaluation of the Corrosion Durability of Steel Systems for
Transcription
Evaluation of the Corrosion Durability of Steel Systems for
INTRODUCTION The Strategic Alliance for Steel Fuel Tanks (SASFT) was organized in 2000 by the American Iron and Steel Institute (AISI) to bring together the diverse business disciplines involved in designing, manufacturing and supplying steel fuel tanks in the automotive market. SASFT has evolved to become an international alliance of 32 companies having a common interest in the development, optimization and application of fuel tanks for automobiles. The full members are shown on the back page of this report, along with those automobile OEM Associate members who participate in an advisory capacity. The corrosion study reported herein was organized, managed and written by the Corrosion Evaluation Team of SASFT. The participating companies and individual representatives of the Corrosion Evaluation Team were as follows: For More Information on SASFT: Visit: www.sasft.org Contact: Peter Mould Program Manager 001 810.225.8250 [email protected] For More Information on AISI: Visit: www.autosteel.org Contact: Ronald Krupitzer Senior Director 001 248.945.4761 [email protected] Arcelor Laurent Dallemagne Gerd Schwerzel Michel Luciani Art Coleman Corus Terry Burton Dofasco, Inc. Rick Daley Harley Davidson Sue Jokela International Steel Group Steve Jones Stavros Fountoulakis JFE Steel Setsuo Mega Tetsuo Sakiyama Toshihiro Kikuchi Martinrea International Ray Sheffield National Steel Corp. Bruce Hartley Nippon Steel Shinichi Itonaga The Magni Group Doug Paul (Chairman) Greg Tarrance ThyssenKrupp Stahl Wilhelm Warnecke United States Steel Corp. Matt McCosby SASFT's global reach recognizes that different business and technological issues impact the type of fuel tanks produced in different geographic regions. By understanding these issues rational, optimized approaches can be fully deployed for steel fuel tanks. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks -2- TABLE OF CONTENTS Introduction ....................................................................................................................................................................................... 2 Executive Summary .......................................................................................................................................................................... 4 Genesis of the Corrosion Study ....................................................................................................................................................... 6 Historical Assessment of the Corrosion Resistance of Steels for Automobile Fuel Tanks ...................................................... 7 Scope and Objectives of the Corrosion Study ................................................................................................................................ 8 General Considerations of Corrosion Testing for the SASFT Study Test approach and input from automakers ................................................................................................................................... 9 Exposure times and life equivalencies ........................................................................................................................................... 9 Steel system candidates for corrosion testing ............................................................................................................................. 10 Criterion for failure ......................................................................................................................................................................... 11 Independent testing ........................................................................................................................................................................ 11 Experimental Procedures Adopted for the Corrosion Study Test methods and corrosion evaluation procedures .................................................................................................................. 13 - Neutral Salt Spray (ASTM B117) - Cyclic Corrosion Resistance Test (SAE J2334) - Test validation specimens - Gravelometer - Fuel Test Configuration and Preparation of Test specimens ..................................................................................................................... 14 - Specimens for External Testing (Neutral Salt Spray and Cyclic tests) - Specimens for Internal Testing (Fuel tests) - Fabrication of Test Specimens Evaluation Procedures ................................................................................................................................................................... 18 - Neutral Salt Spray test - Cyclic Corrosion test - Gravelometer test - Fuel test Test materials (steel systems) ........................................................................................................................................................ 20 Results and Discussion External Neutral Salt Spray test (ASTM B117) ............................................................................................................................ 22 - Qualitative Evaluation after 2000 hours - Quantitative Evaluation External Cyclic Corrosion Resistance Test (J2334) ..................................................................................................................... 25 - Qualitative Evaluation after 80, 120 and 160 cycles - Quantitative Evaluation Internal Fuel Test ............................................................................................................................................................................ 32 - Qualitative Evaluation - Quantitative Evaluation Summary of Results ........................................................................................................................................................................ 37 Conclusions ..................................................................................................................................................................................... 43 References and Notes ..................................................................................................................................................................... 44 Acknowledgments .......................................................................................................................................................................... 45 List of Attachments ........................................................................................................................................................................ 46 - Photo Library (file names, photo and specimen identifications) .................................................................................... 48 - Appendixes ............................................................................................................................................................................ 57 - Listing 1: Neutral Salt Spray ............................................................................................................................................ 48 - Listing 2: Cyclic Corrosion ............................................................................................................................................... 50 - Listing 3: Fuel Test ............................................................................................................................................................. 54 - SASFT Members ..................................................................................................................................................................... 90 Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks -3- EXECUTIVE SUMMARY In recent years, automakers have questioned the corrosion durability of steel for automotive fuel tanks. To address this concern, the Strategic Alliance for Steel Fuel Tanks (SASFT), an international group of 32 companies representing steel fuel tank manufacturers, suppliers and steel companies, and organized by the American Iron and Steel Institute (AISI), sponsored a comprehensive study of the corrosion resistance of several commercially available steel systems. The objective of the corrosion study was to assess the resistance of selected steels to the severe external corrosion conditions experienced by automobile fuel tanks and to the potential for internal corrosion (inside the fuel tank) posed by aggressive alcohol-containing fuels. It was particularly important to assess the ability of the steels to meet the 15-year durability requirements set by the California Air Resources Board (CARB) for low emission vehicles. In recent years, various new steel "systems" have been developed by the worldwide steel industry for automobile fuel tanks. (The term "system" denotes a unique approach for resisting corrosion, such as special coatings, and/or special steel alloys.) Twelve of these systems were initially selected for this study by SASFT. However, 2 post-painted systems were subsequently withdrawn because of inadequate paint film thicknesses. Thus, 10 steel systems completed the testing in this study. The steels selected were representative of the three principal categories of steel tank manufacturing approaches currently used throughout the world; these are: Pre-painted steels: Tanks are manufactured from steel coils which have been pre-painted on both sides of the steel sheet. The assembled tanks then receive limited, local post-painting on the outer surfaces at the weld areas. Post-painted steels: Steel tanks are fabricated from unpainted steel coils. The tanks are then post-painted completely on the outer tank surfaces. Bare steels: Bare steels (such as stainless steels) where no pre- or post-painting is used. Test specimens were specially designed to reflect the unique corrosion conditions of a fuel tank affixed to a vehicle. The External Corrosion specimens incorporated a scribe line to simulate a scratch exposing the bare steel, a dome simulating forming strains, a weld flange with a clip to simulate a crevice corrosion site, and an area exposed to gravel impact which simulates stone chipping conditions. To assess the External Corrosion resistance, two simulative bench-scale procedures were used: the Neutral Salt Spray test (ASTM B117) with exposures up to 2000 hours and the Cyclic Corrosion test (SAE J2334) with exposures up to 120 and 160 cycles. The latter exposures were selected to simulate road lives of 15 years and 20 years, respectively. Perforation was adopted as the criterion for failure. However, the progress of corrosion was assessed qualitatively by visual observation and photographs, and quantitatively by measuring pit depths over the entire specimen, assessing coating integrity by creepback at the scribe line and chip ratings after gravel impact. To determine the Internal Corrosion resistance, deep drawn cups and flat lids were assembled to contain an aggressive fuel (CE10A). (This fuel was chosen on the basis of prior experience by automakers and their recommendations to SASFT.) The fuel- cup assembly was sealed by an inert gasket and clamping rings. The fuel cup assemblies were held at 45 ± 2°C for 39 weeks to simulate a 15-year tank exposure. The fuel was changed every four weeks to simulate repeated fuel tank filling and to replenish contaminant ions and minimize oxygen depletion (per the test fluid specifications of SAE J1747). The extent of corrosion was evaluated qualitatively by recording the extent and location of corrosion and quantitatively by weight changes and pit depths. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks -4- EXECUTIVE SUMMARY (Cont.) The following key findings were obtained from the two External Corrosion tests: No perforation was observed at any location for any of the steel systems. Corrosion pit depths were observed at isolated locations for only two steels. Additionally, the maximum depths of the pits were only 0.2 to 0.4mm, representing about 20 to 40 percent of the original steel thickness. The extent of corrosion (red and white rusting) varied by location on the specimen and from material to material. For the most part, slight (<15% surface area) or moderate (15-30%) rusting was observed, and pronounced rusting (>30%) occurred only in a few instances. The variations in the extent of corrosion were not of such significance to rate one steel system over another. The integrity of the paint systems, as indicated by resistance to gravel impact and creepback, varied in proportion to the thickness of the paint films. Those pre-painted systems having thin organic resin films (about 9µm thick) and one stainless steel, having an inorganic paint film (about 17µm thick), showed small amounts of paint chip loss after initial gravel impacts. However, subsequent gravel impacts did not progressively increase the paint chip loss. Those post-painted systems having thick coatings (up to 370µm) showed no paint chip loss or creepback at the scribe line. Steels with thin post-paint films (20 to 150 m) showed adhesion loss and creepback proportional to the coating thicknesses. This suggests that the paint integrity of these systems could be increased by using thicker paint films. The results for the Internal Corrosion (Fuel) tests showed: Very minor weight losses (less than 0.13%) for all the specimens after the maximum 39-week exposure. Some variations in the extent of a white residue occurred between the samples. The white residue occurred primarily at the liquid-vapor interface. However, the residue was insufficient to conduct any post exposure analysis. No perforation occurred and, in fact, no pits deeper than 0.1mm were observed in any of the cups or lids. The results demonstrate that all of the steel systems tested in this bench-scale study will resist external and internal corrosion (in the severe environments that can be experienced by automotive fuel tanks) for up to 20 years. Thus, it is fully expected that the systems will meet the 15-year durability requirements of CARB. It is recommended that automakers conduct their own tests (including proving ground tests) to validate the on-vehicle corrosion durability of the steel systems tested herein. The selection of one steel system over another will depend on factors other than the corrosion resistance, such as the manufacturing approach favored by the automaker, material and manufacturing costs, inherent manufacturability (forming and welding), and available manufacturing equipment. Because these factors are beyond the scope of this study, it is recommended that automakers contact the suppliers of the specific steel systems. The guidance and encouragement received from many automakers during the development of the testing methodology used in this study is gratefully acknowledged. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks -5- GENESIS OF THE CORROSION STUDY Steel has been the material of choice globally for automobile fuel tanks for the majority of the 20th century. The steel used primarily has been low carbon steel, coated with a terne alloy (90% lead and 10% tin). The terne coating was an effective barrier to potential corrosion from the external environment (road salts, stone chipping, etc.) and the internal environment (gasoline and diesel fuels). Despite the long, successful history of terne-coated steel fuel tanks, the following business and technical issues have caused a significant change in fuel tank materials and in the type of steel for the steel option. Legislative pressures to reduce heavy metals in the manufacturing and recycling streams. This caused automakers to move away from lead-containing materials including terne-coated sheet steel. Automaker requirements for increased durability as a result of more severe corrosion environments such as increased usage of road salts as well as the emergence of flexible fuels. Emergence and growth of highly durable HDPE plastic fuel tanks. Legislative regulations on automobile evaporative emissions to reduce air pollution. Several national government agencies (such as U.S. EPA and equivalent organizations in Europe and Japan) have set maximum emission levels for light vehicles (cars and light trucks). In the U.S.A., California's Air Resources Board (CARB) has set very strict emission levels to reduce California's acute air pollution problems. Because of steel's inherent impermeability to fuels, steel tanks are well-suited to meeting California's stringent evaporative emission standards. However, an additional requirement by CARB, for 15-year durability of the exhaust emission system and the entire fuel system raises the issue of the corrosion resistance of the materials used. In response to the demand for more durable steels for fuel systems, steel makers worldwide developed a variety of new steel "systems," where "system" describes a compound approach to achieving good corrosion resistance while retaining good manufacturability (forming and welding) and tank performance. Such systems include, metallic coated low carbon steels with sophisticated pre-paints and post-paints, as well as stainless steels (such as austenitic 304L and ferritic 436L steels), and are commercially available. The durability of the commercially available steel systems has been assessed by steel companies and users alike. However, a variety of corrosion tests, sometimes company specific, were used to assess durability. Additionally, from these tests it was not apparent that the exposure times equated to a 15-year service life. This situation prompted the need to determine the corrosion resistance of the new steel systems using standard test protocols that would indicate a 15-year service durability and was the genesis for the corrosion study conducted by the Strategic Alliance for Steel Fuel Tanks (SASFT). Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks -6- HISTORICAL ASSESSSMENT Historically, a three-stage process has been used to assess the corrosion performance of steel for fuel tanks. Bench Scale Simulative Corrosion Tests These tests are conducted by steel suppliers and automakers alike. The tests are used primarily as screening tests for further evaluation in full scale proving ground tests. Of the many tests that have been used in the past, three of the most commonly used are a Neutral Salt Spray corrosion test (ASTM B117) which exposes test strips or coupons to a continuous salt spray for a fixed time at a specified temperature, a Cyclic corrosion test (SAE J2334) having prescribed cycles of exposure to salt spray and dry times at specified temperatures for various times (cycles), and various Fuel Resistance tests where company-preferred tests are used for any fuel of interest. Because of the concern regarding how well simulative tests relate to actual on-vehicle performance, additional proving ground tests are always conducted by all automakers. Automotive Proving Ground Tests Each automaker has its own prescription for assessing the corrosion resistance of fuel tanks. Common features are formed tanks or shells and/or panels fixed to a sled or installed on a vehicle, which is driven over a track while undergoing a 'menu' of exposures to salts, dry periods and gravel. Field Surveys of Actual Vehicles Corrosion surveys of actual in-service vehicles (after 5 years, 10 years, 15 years, etc.) are conducted regularly in areas of severe corrosion (such as the northeast of U.S.A., Florida or the maritime provinces of Canada). These surveys evaluate the actual extent of corrosion of fuel systems, body structures and body panels and validate proving ground tests and, to some extent, bench scale simulation tests. From the above assessments automakers are able to establish correlations. However, the predictability of bench scale simulative tests is not sufficiently accurate to avoid conducting proving ground tests. Thus for steel fuel tank materials, the durability performance assessment varies according to the assessment method as follows: Assessment Method Performance Predictability Bench scale simulative tests Proving ground tests Field surveys of corrosion on vehicles Indication only Good measure of performance Validation Because SASFT did not have the capability to conduct proving ground tests and it was premature to conduct field surveys because of the 'newness' of many steel systems, SASFT decided to conduct bench scale simulative tests. It was envisioned that these tests, although only indicative of long-term service durability, would provide encouragement for automakers to conduct their own proving ground tests for the various new steel systems. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks -7- SCOPE AND OBJECTIVES Scope - It was regarded as important to adopt a broad scope with respect to the selection of steel systems for corrosion testing - regardless of the regional origin of the steel systems. Because regionally-developed steel systems can be migrated to other regions, several steel "options" can be considered by automakers for 15-year-life fuel tanks. The detailed analysis of costs, manufacturability and performance could be determined subsequently by interaction between the individual steel companies, tank manufacturers and automakers. A somewhat narrower scope was adopted in selecting the corrosion tests: The external tests were of recognized value primarily to North American automakers and suppliers. But specific unique features were incorporated to reflect actual conditions experienced by an automobile fuel tank rather than by body panels or body structures. The internal fuel test selected was uniquely designed by SASFT, based on existing tests in Europe and in Japan. Objectives - The following objectives were established for SASFT's corrosion study: Select suitable steel systems (available from worldwide steel industry) for meeting a 15-year life. Select suitable bench-scale tests for assessing the durability performance of steels in an automotive fuel tank environment; specifically external corrosion resistance (resistance to salts, stone impingement, etc.) and internal corrosion resistance to aggressive fuels. Obtain feedback from automakers on the value of the SASFT corrosion program before the tests were started. In this way, the results would be meaningful to automakers. Conduct the tests at an independent test laboratory (outside of the SASFT and AISI organizations). Share the results with automakers and encourage their further evaluation of the steel systems using proving ground or other tests. To accomplish these objectives, a Corrosion Evaluation Team was formed which organized and managed the program. The effectiveness of the team was enhanced by the ability of company representatives to draw from the resource bases of their companies. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks -8- GENERAL CONSIDERATIONS Testing Approach Because of a lack of access to proving grounds and their infrastructure, SASFT decided to use established accelerated bench scale corrosion tests. Several tests were considered by the Corrosion Evaluation Team; two external tests and one internal test were selected. Neutral Salt Spray Test (ASTM B117) The CET was aware that there is a poor correlation of results from this test with actual perforation corrosion of fuel tanks or body panels in proving ground tests or field surveys. However, because of the wide use of the test and the large availability of data from other test programs, it was decided to include the test. Furthermore, it was seen as valuable to determine whether any correlations could be made with the results of the preferred external test, i.e. the Cyclic Corrosion Test (SAE J2334). Cyclic Corrosion Test (SAE J2334) Much work has been conducted on this test by the SAE J2334 Committee over the last 20 years. This has culminated in recent papers indicating the value of the test as a practical means for assessing perforation corrosion resistance [1 - 4]*. Information on the predictability of the J2334 Cyclic Corrosion test is reproduced from one of the referenced papers in APPENDIX 1. Currently, the J2334 cyclic corrosion test is generally regarded as a useful simulative bench test for predicting perforation performance in subsequent proving ground tests or in actual vehicle performance. Therefore, SASFT selected the base J2334 test for evaluating the various steel systems. However, modifications to the test procedure were incorporated to better represent the external conditions experienced by fuel tanks. These include: - a unique test specimen containing: - a welded flange - a plastic clip on the welded flange to provide potential crevice corrosion sites - a scribe line simulating scratching down to bare steel - a dome to simulate the formed areas of a fabricated steel tank - a procedure for simulating gravel impact on a tank by using the standard SAE J400 Gravelometer Test on a flat portion of the specimen. Internal (Fuel) Corrosion Test Features and elements of existing fuel corrosion resistance tests developed by Corus (Europe) and JFE Steel (Japan) were incorporated into a SASFT designed, sealed cup test. The selection of aggressive fuel CE10A was chosen on the basis of findings from a cooperative survey conducted by the Big 3 automakers of the 'aggressiveness' of a variety of fuels. From this survey, CE10A was found to be a very agressive fuel. To ensure that the results from the SASFT corrosion test program would be valuable to automakers, the original proposed tests, test specimens, test procedure and steel systems were reviewed with key engineering personnel at automakers worldwide. As a result of feedback and suggestions, several modifications were incorporated into the original SASFT test program. Exposure Times and Life Equivalencies For the Neutral Salt Spray Test, SASFT was unaware of any correlation between exposure time and equivalent corrosion in a vehicle. Because North American auto manufacturers generally use exposure times of 1,000 to 2,000 hours, SASFT decided to use a 2,000-hour exposure time. For the Cyclic Corrosion Test, SASFT learned from various corrosion experts that 80 cycles is generally regarded as being approximately equivalent to 10 years vehicle life on the basis of correlations between cyclic testing, automotive proving ground tests and field * see references and notes at the end of this report. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks -9- GENERAL CONSIDERATIONS surveys. Assuming a linear relationship between the number of cycles and life equivalency, 120 cycles should represent 15 years. SASFT decided to run the Cyclic Corrosion Test beyond 120 cycles (15 years) and complete the exposure after 160 cycles (20 years). For the Fuel Corrosion Test exposures of 26 weeks to various fuels at 45°C are used by some automakers to represent performance of an actual fuel tank after 10 years. Consequently, the exposure test period was increased by 50% to simulate 15-year tank exposure. The exposure times and life equivalency are summarized in EXHIBIT 1. Exposure Times Typically used by N.A. Automakers Neutral Salt Spray Test (ASTM B117) 1000 to 2000 hours Cyclic Corrosion Test (SAE J2334) 80 cycles SASFT Exposure, Time 2000 hours 160 cycles 26 weeks Fuel Test 39 weeks Approximate Life Equivalency (years) —— —— 10 years 20 years 10 years 15 years EXHIBIT 1. Exposure times and life equivalency for various corrosion tests. Steel System Candidates for Corrosion Testing The global nature of SASFT's membership, particularly with respect to steel companies, enabled a broad survey of candidate steel systems for corrosion testing to be conducted. Furthermore, the list of candidate steel systems reflected the different preferred approaches to steel selection and tank manufacturing in different geographical regions as shown in EXHIBIT 2. Geographic region North America Big Three Transplants Europe Japan/Korea Preferred steel manufacturing approach for automobile fuel tanks Pre-painted steel and limited post-painting Post-painting of assembled tanks Bare steels (HD Aluminized* and stainless) and post-painting of HD Aluminized and stainless Post-painting of assembled tanks *Used largely by DaimlerChrysler (Mercedes) for tanks placed above the floor pan and not exposed directly to road salts. EXHIBIT 2. Preferred steel types and manufacturing methods for automobile fuel tanks by geographical region. An additional factor in selecting steel materials was a need to evaluate and compare the performance of materials containing Cr+6 with those that are Cr+6 free. As a result of the above considerations, 12 steel systems were chosen initially for the corrosion study. However, 2 post-paint systems were subsequently withdrawn because of incorrect paint thicknesses. The remaining 10 systems and the suppliers of the test materials are shown in EXHIBIT 3. (More complete details of the steel systems are described under test materials in the subsequent section entitled “Experimental Procedures Adopted.”) Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 10 - GENERAL CONSIDERATIONS Category Prepainted steels ID No. 1 Other coating Presence of Cr +6 ISG (Bethlehem) Epoxy pre-paint water-based postpaint at welds Yes ISG (Bethlehem) Epoxy pre-paint water-based postpaint at welds No U.S. Steel (National) Epoxy pre-paint water-based postpaint at welds No 4 Low carbon steel/ HD Aluminized Aℓ-Si** ThyssenKrupp Stahl Epoxy pre-paint water-based postpaint at welds Yes 5 Austenitic 304L stainless/ None Low carbon steel/ HD Terne Pb-Sn Arcelor (J & L Specialty)* Inorganic coating No Nippon Steel Corp. Acrylic and top coat post-paint (external surface only) No 7 Low carbon steel/ HD Tin Zinc (Sn-Zn) Nippon Steel Corp. Acrylic and top coat post-paint (external surface only) No 8 Low carbon steel/ HD Aluminized Aℓ-Si Arcelor Alkyd resin synthetic polymer postpaint (external surface only) Yes 9 Ferritic 436L stainless/ None JFE Steel Zinc-rich paint (external surface only) No 10 Austenitic stainless/ None Arcelor (J & L Specialty)* None No 3 Bare steels Supplier of steel samples‡ Low carbon steel/ Electrogalvanized Zn-Ni Low carbon steel/ Electrogalvanized Zn-Ni Low carbon steel/ HD Galvannealed Zn-Fe 2 Postpainted steels Steel System Base steel/Metallic coating 6 304L ‡ The same steels may be available from other steel companies. * Now part of Allegheny Ludlum. ** Subsequently referred to as HD Aluminized or HDAℓ EXHIBIT 3. Steel systems selected by SASFT for external and fuel corrosion testing. Criteria for Failure and Extent of Corrosion Because the prime function of a fuel tank is to contain fuel, perforation of the test specimen was adopted as the criterion for failure. Additionally, various qualitative and quantitative assessments of corrosion were used to indicate the progress of corrosion up to the point at which perforation (failure) occurs. It was expected that the progress of corrosion might differ from region-to-region on the specimen because of the different conditions in the specimen such as forming deformation, scratches, weld zones, and gravel impact zone. Therefore, in the External Tests corrosion assessments were made at several locations of the test specimens which simulated different tank conditions (described later under Configuration and Preparation of Specimens in the section Experimental Procedures Adopted). For the Internal Corrosion Tests the extent of corrosion and pitting was assessed at several locations (liquid contact, liquid-vapor interface, and vapor contact areas at the cup side walls and lids). In this way, the specific 'corrosiveness' of the liquid fuel, liquid-vapor interface (including phase separation of the fuel) and vapor could be determined. Independent Testing Although excellent corrosion testing facilities were available in many member companies of SASFT, it was decided to contract the testing with a reputable testing laboratory whereby the testing and interpretation of results is entirely independent of SASFT and its members. Accordingly, several testing laboratories with experience in automotive corrosion testing were surveyed. After careful review, ACT Laboratories, Hillsdale, Michigan, were contracted to conduct both the external corrosion testing and the fuel testing. Key factors which merited the selection of ACT Laboratories were: Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 11 - GENERAL CONSIDERATIONS Excellent capabilities in automotive corrosion testing. Good reputation with the automotive community (OEMs and suppliers). Extensive prior involvement with SAE J2334 committee in developing and validating the Cyclic Corrosion Test. Accessible laboratories in Hillsdale and Wixom, MI. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 12 - EXPERIMENTAL PROCEDURES ADOPTED Test Methods Details of the test procedures are described as follows: Neutral Salt Spray Test The test was conducted according to ASTM B117 [5]. Key process parameters were: - Continual atomized spray (or fog) of 5% salt solution in an enclosed chamber. - Temperature of chamber: 35ºC. - Triplicate specimens were spaced from each other and inclined at 15º from vertical. - Maximum exposure time of 2000 hours. - Gravel impact was conducted according to SAE J400 at the start of testing and after 500, 1000, and 1500 hours of salt spray exposure. Cyclic Corrosion Test The test was conducted according to SAE J2334 procedures [6]. Key process parameters were: - One 24-hour cycle in an enclosed chamber included: - 6 hours exposure in 100% condensing humidity at 50°C (+ 2°C). - 15 minutes exposure at 25°C to a salt solution consisting of, 0.5% NaCl, 0.1% CaCl2 and 0.075% NaHCO3. - 17.75 hours exposure in a dry stage (60°C + 2°C, 50% + 5% relative humidity). A schematic of the daily cycle is shown in EXHIBIT 4. - Duplicate specimens were spaced from each other and inclined at 15° from vertical. - Gravel impact was conducted according to SAE J400 at the start of testing and after 20 cycle intervals. Separate sets of specimens were used for 80-, 120-, and 160-cycle exposures. - Six coupons of bare cold-rolled steel were included in the Cyclic Corrosion test for the purpose of assessing weight loss and perforation for an uncoated steel (no metallic coating and no pre- or post-paint.). Humid Stage 6 hr. 50 C, 100% RH Salt Dip 25 C, 15 min. 0.5% NaCl + 0.1% CaCl2 + 0.075% NaHCO3 Dry Stage 60 C, 50% RH Daily Dry Stage 17 hr., 45 min. Weekends and Holidays 60 C, 50% RH EXHIBIT 4. Daily cycle for the Cyclic Corrosion Test (SAE J2334). Test Validation Speciments To ensure that the test conditions in both the Neutral Salt Spray and Cyclic corrosion tests were stable within the duration of the tests and consistent with previous tests, test validation specimens of pure zinc and uncoated steel sheet were incorporated in the test chambers. Weight loss of the coupons was recorded as follows: Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 13 - EXPERIMENTAL PROCEDURES ADOPTED Exposure, time/cycles Neutral Salt Spray Test 500 hrs. 1000 hrs. Cyclic Corrosion Test 80 cycles 120 cycles 1500 hrs. 160 cycles 2000 hrs. —— Gravelometer Test The test used in both the Neutral Salt Spray Test and the Cyclic Corrosion Test was conducted according to SAE J400 (Revised 2002-11) [7]. Key process parameters were: - A QGR gravelometer was used. - Room temperature and an air pressure of 70 + 3 psi. - 1 pint of water-worn road gravel that passes through a 16mm (5/8 inch) space screen, but retained on a 9.5mm (3/8 inch) space screen. - The gravel was aimed to impinge only on the target area immediately below the weld flange. Fuel Test The test fuel used was CE10A and constituted, in accordance with SAE J1681, [8] as follows: - For 1 liter of Test Fuel (CE10A): 450 milliliters of Toluene 450 milliliters of iso-Octane 100 milliliters of Aggressive Ethanol - Aggressive Ethanol: 816.0 grams (1.034 liters) of Denatured Ethanol, CDA 20 8.103 grams (8.1 milliliters) of ASTM D 1193 - Type II Water 0.004 grams of Sodium Chloride 0.021 grams (11 microliters) of Sulfuric Acid 0.061 grams (58 microliters) of Glacial Acetic Acid The test cups and lids (described later in Specimens for Internal Testing) were cleaned with warm water, dried and weighed before adding 30 ml of the test fuel, which half-filled each cup. The assembled fuel test cups were placed in a sand bath controlled to 45 ± 2°C according to the test procedures of SAE J1747 [9]. Total exposure time for the stationary fuel test assemblies was 39 weeks to simulate a 15-year fuel tank exposure. To simulate regular and re-filling of a fuel tank and to replenish contaminant ions and minimize oxygen depletion (per SAE J1747). Each fuel test assembly was removed from the sand every four weeks, the fuel was removed and saved, the cup and lid reweighed, new fuel added and the assembly returned to the sand bath. The spent fuel was checked for any discoloration. Configuration and Preparation of Test Specimens Specimens for External testing (Neutral Salt Spray and Cyclic tests) Historically, for bench scale corrosion testing of steel, the test specimens have been flat coupons with some form of edge protection (tape or stop-off paint). In some cases the specimens might contain a scribe line and a dome to simulate a scratch and forming strains, respectively. The Corrosion Evaluation Team of SASFT felt that the test specimen for this study ought to represent more fully the conditions experienced by steel in an assembled fuel tank. Accordingly, the unique test specimen shown in EXHIBIT 5 was developed for both of the external corrosion tests. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 14 - EXPERIMENTAL PROCEDURES ADOPTED Olsen dome 6 inches Weld 6 inches Plastic Clip scribe line (applied at test laboratory) 4 inches gravel impact zone 2 inches max. flange width EXHIBIT 5. Specimen configuration for both External Corrosion tests Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 15 - EXPERIMENTAL PROCEDURES ADOPTED The 4-inch wide test specimen included: - an Olsen dome to simulate forming strains. The 22.22mm (7/8th inch) diameter dome is formed to a depth of 7.9mm (0.3 inch). The domes were introduced into the steel specimens according to ASTM E643-84 (Re-approved 2000). [10] - a scribe line such that the bare steel is exposed to simulate a severe scratch. The scribing was conducted according to ASTM D1654 - 00 [11] using a straight shank lathe tool (style E). - a welded flange area to simulate the electric resistance seam weld of a steel fuel tank. - a plastic clip to provide potential crevice-corrosion sites. - a gravel impact zone for simulation of frequent over-the-road stone chipping. All test specimens were protected at the cut edges by a stop-off paint (Microstop). A photograph of a test specimen is shown in the inset in EXHIBIT 5. Specimens for Internal Testing (Fuel tests) A unique sealed fuel test cup was developed and used for the fuel resistance tests. 50 mm diameter cups were drawn to a depth of 30 mm with a residual cup flange. The cup was half filled with 30 ml of the test fuel so that the cup was exposed to the fuel and vapor while the lid was exposed only to the vapor. To seal the fuel and vapor, a 1/8 inch thick Viton® flange gasket [12] was placed on top of the flange surface of the cup, the lid positioned and clamped by upper and lower ¼ inch thick steel clamping rings secured with 4 equally spaced bolts [13]. A torque wrench was used to apply a fixed torque of 1.1 Newton-meter (10 inch-pounds) to each of the 4 bolts. The fuel test components (including the torque wrench) are shown in EXHIBIT 6. A schematic representation of the fuel test assembly and a photograph of the assembly are shown in EXHIBITS 7 and 8, respectively. EXHIBIT 6. Components of the fuel test unit: torque wrench, fuel-containing cup, Viton® gasket seal, steel sample lid, bottom clamping ring, top clamping ring and the combined lid plus top clamping ring. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 16 - EXPERIMENTAL PROCEDURES ADOPTED Viton Gasket seal 4 Clamping bolts Steel sample for lid Circular steel clamping rings 30mm Drawn sample cup Fuel 50mm Blank diameter Punch diameter Die radius Clamping torque Draw depth = = = = = 98 mm 50 mm 3 mm 1.1 newton-meter (10 inch pounds) 30 mm EXHIBIT 7. Schematic of the fuel test assembly fully immersed in a temperature-controlled sand bath. To maintain a constant temperature of 45± 2°C, the fuel test assemblies were placed in a controlled temperature 10 inch (254 mm) deep sand bath. The test assemblies remained stationary for each 4-week exposure. EXHIBIT 8. Profile of an assembled test cup unit. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 17 - EXPERIMENTAL PROCEDURES ADOPTED Fabrication of Test Specimens Flat steel-system sheets were supplied by various steel companies to a target thickness of 1mm (0.0395 inch). For External Corrosion test specimens, the various sheets were welded, either by using a conventional seam welding technique, or by a Soudronic process using production welding practices. The welded specimens of pre-painted steels were post-painted at the weld zone. All welded specimens were gathered at Bethlehem Steel Corporation (now International Steel Group) where the Olsen domes were formed. All specimens were then shipped to ACT Laboratories where any forming lubricants were removed by light washing and the scribing and edge painting was completed before testing. For Internal Corrosion test specimens, all the fuel cups were deep drawn and the flat lids cut at Bethlehem Steel using the same uniform procedures for each material. The specimens were then shipped to ACT Laboratories for cleaning, drying and assembly with gaskets. Evaluation Procedures External - Neutral Salt Spray Test The qualitative evaluation of Neutral Salt Spray specimens was conducted at every 500 hours before and after air drying and cleaning by blowing air at 80 psi at an angle of approximately 45º over the entire specimen surface. The specimen surface was lightly contacted with the air nozzle to clean the surface by removing loosely adherent coatings. Each of the triplicate specimens was visually examined for corrosion and loss of adhesion at the scribe line, chipped (graveled) area, Olsen dome, flange (including weld and clip locations) and field area (region above the dome). The extent of corrosion was rated according to the following scale and assigned a numerical rating as follows: Corrosion Severity Numerical Rating N = None: No corrosion 0 S = Slight: Approximately less than 15% corrosion in test area 1 M = Moderate: Approximately 15 - 30% corrosion in test area 2 P = Pronounced: Approximately greater than 30% corrosion in test area 3 The quantitative evaluation of the Neutral Salt Spray specimens was conducted at the completion of testing (i.e., after 2000 hours) by four methods: - Weight loss. - Creepback from scribe line. The distance of the affected paint film (lost or non-adherent) between the scribe line and the unaffected paint film was reported as: - Average: The average of 6 measurements of creepback from the scribe at points 10mm apart centered on the scribe line. Each measurement was an average of the creepback on two sides of the scribed line. - Maximum: A measurement of the creepback from the scribe line at the point having the most extensive amount of affected paint, but discounting those areas less than 1cm from the ends of the scribe line. - Minimum: A measurement of the creepback from the scribe at the point with the least extensive amount of affected paint, but discounting those areas less than 1cm from the ends of the scribe line. - Pit depth. Maximum pit depth (greater than 0.1mm, which is approximately 10% of the initial specimen thickness) was measured for each specimen after 2000 hours. - Chip rating. The test method and evaluation procedure is described below under the Gravelometer Test method. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 18 - EXPERIMENTAL PROCEDURES ADOPTED A summary of the qualitative and quantitative assessments for the Neutral Salt Spray test is shown in EXHIBIT 9. 500 Qualitative Photographs Before cleaning After cleaning Visual assessment After cleaning Quantitative Creepback Pit Depth Chip rating Exposure time, hours 1000 1500 2000 √ √ √ √ √ √ √ √ √ √ √ √ —— —— √ —— —— √ —— —— √ √ √ √ EXHIBIT 9. Qualitative and quantitative assessment of corrosion in the Neutral Salt Spray test. External - Cyclic Corrosion Test A qualitative evaluation was conducted after every 20 cycles by visually assessing, after air blowing but without cleaning, the extent of corrosion and loss of any coating adhesion at the scribe line, chipped (graveled) area, Olsen dome, flange (including weld and clip locations) and field area (region above the dome). The extent of corrosion or adhesion loss was rated the same way for the Neutral Salt Spray specimens. The specimens were also photographed. The quantitative evaluation was conducted after 80 cycles, 120 cycles and 160 cycles of exposure. The specimens were air dried and cleaned using 80 psi air pressure at a 45° angle over the entire specimen surface. The specimen surface was lightly contacted by the air nozzle to remove loosely adherent coatings. Weight loss, creepback, pit depth, and chip ratings were assessed in the same way as for the Neutral Salt Spray test. A summary of the qualitative and quantitative assessments for the Cyclic Corrosion test is shown in EXHIBIT 10. 60 Qualitative Evaluation Remove specimens temporarily and without cleaning: ― assess corrosion damage according to ASTM D610 ― take photographs Quantitative Evaluation Remove specimens permanently,* clean and then: ― weigh ― assess creep back ― determine pitting location and depth No. of Cycles (life equivalency) 80 100 120 140 (10 years) (15 years) 160 (20 years) √ √ √ √ √ √ √ √ √ √ √ √ —— —— —— √ √ √ —— —— —— √ √ √ —— —— —— √ √ √ * Separate sets of specimens were used for 80-, 120-, and 160-cycle exposures. EXHIBIT 10. Qualitative and quantitative assessment of corrosion in the Cyclic Corrosion test. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 19 - EXPERIMENTAL PROCEDURES ADOPTED Gravelometer Test The evaluation procedure used was based on visual comparison of the test specimens with SAE J400 pictorial standards. A number-letter combination in which rating numbers 10-0 indicate the number of chips of each size and rating letter A-D designate the sizes of the corresponding chips. The codes are described fully with the tabulated results in subsequent EXHIBITS and APPENDIXES. Additionally, the nature of failure was noted as to whether adhesion loss occured from the metallic coating to topcoat or from the steel substrate to topcoat. Internal Fuel Test The qualitative evaluation was conducted by inspecting the fuel test cups and lids after each fuel change and assessing of the extent of corrosion. The same visual rating scale was used as for the external tests. The quantitative evaluation was conducted by measuring the weight loss (change) and the extent, location and depth of pits. Test Materials (steel systems) The steel systems used for External Corrosion testing are shown in EXHIBIT 11, together with a description of the external surfaces exposed to the corrosion environments. Coatings on both sheet surfaces I.D. Number Base Steel Metallic Coating/Coating weight per side Exterior Surface Post-paint thickness Sheet Thickness mm* Pre-treatment /thickness Pre-paint/ thickness Magni 331 +6 with Cr epoxy /9.5 µm Magni 336 +6 non- Cr epoxy /9.5 µm Weld only Magni W46 / 127µm (both sides of flange) Magni 336 +6 non- Cr epoxy /9.5 µm Magni 369 +6 with Cr epoxy /9µm Neukote inorganic coating / 17µm Weld only Magni W46 / 127µm (both sides of flange) None Anti chip acrylic /350µm + Pre-painted steels 1 Low carbon (IF) steel Electrolytic Zn-Ni /30 g/m2 1.07 2 Low carbon (IF) steel Electrolytic Zn-Ni /30 g/m2 1.07 3 Low carbon (IF) steel Hot dip galvannealed (Zn-Fe) /45 g/m2 0.8 4 Low carbon (IF) steel 0.88 5 Austenitic Stainless (304L) Hot dip aluminized (Al-Si) /30 g/m2 None 0.89 Bonderite 1303 mixed oxide with Parcolene 62 Cr+6 rinse / 92 10mg/m Bonderite 1303 mixed oxide with Parcolene +6 350 non- Cr rinse /910mg 2 /m Bonderite 1303 mixed oxide with Parcolene +6 350 non- Cr rinse /92 10mg/m Bonderite 714 with +6 Parcolene 62 Cr rinse None Hot dip terne (PbSn) /40 g/m2 Hot dip tin-zinc (Sn-Zn) /40 g/m2 Hot dip aluminized (Al-Si) /55 g/m2 None 0.8 Phosphate /3 mg/m2 0.8 Cr & Cr free resin /300 mg/m2 Chromate (i.e., with Cr+6) None None Anti chip alkyd resin (Helmebath) /150µm 0.8 None None Zinc rich paint/20µm None 0.8 None None Bare Weld only Magni W46 / 127µm (both sides of flange) Weld only Magni W46 / 127µm (both sides of flange) None (Neukote pre-paint only) Post-painted steels 6 7 8 9 Low carbon (DQSK) Low carbon (DQSK) Low carbon (DQSK ) Ferritic stainless (436L) Bare steels 10 Austenitic Stainless (304L) Coverpaint / 20µm 0.9 +3 +6 Anti chip acrylic /350µm + Coverpaint / 20µm *Thickness before pre- or post-painting EXHIBIT 11. Description of the pre-painted, post-painted and bare steels for EXTERNAL CORROSION resistance testing. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 20 - EXPERIMENTAL PROCEDURES ADOPTED In addition to the 10 materials shown in EXHIBIT 11, two other post-painted steel systems were selected for external corrosion testing, but were withdrawn after early testing because of incorrect post-paint thicknesses. Photographs of the initial test specimens for each test material are shown in EXHIBIT 12; the specimens received an initial gravel impact, but no exposure either to Neutral Salt Spray or to the Cyclic test. The different colors and textures reflect the different coatings and approaches to resisting external corrosion. EXHIBIT 12. Photographs of initial test specimens (materials #1-#10) for external corrosion testing. All of the steel systems used in the SASFT study represented products in commercial production by the supplying steel companies. Further information on specific steel systems can be obtained from the supplying steel companies shown in EXHIBIT 4. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 21 - RESULTS AND DISCUSSION External - Neutral Salt Spray Test (ASTM B117) Qualitative Evaluation after 2000 hours of exposure Photographs of all test materials after 2000 hours of exposure are shown in EXHIBIT 13. Additional photographs of initial samples (graveled, but zero exposure time), and after 1000 hours, and 2000 hours exposure are shown in Photo Library - Neutral Salt Spray. The identification of the photos and test specimens are shown in the Photo Library - LISTING 1 at the end of this report. Pre-painted steels #1 #2 #3 #4 #5 Post-painted steels Bare steels #6 #7 #8 #9 #10 EXHIBIT 13. Photographs of test materials after 2,000 hours exposure and before cleaning in Neutral Salt Spray. Detailed visual ratings of the severity of white and red rust at eight different locations of triplicate specimens are shown in APPENDIX 2. The overall numerical ratings are displayed in EXHIBIT 14. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 22 - RESULTS AND DISCUSSION EXHIBIT 14. Average corrosion severity display of the visual ratings of white and red rust after 2000 hours of exposure in the Neutral Salt Spray test. White 'rust' for pre-, and post-painted samples may well be a reaction product with the specific paints. (Numeric Corrosion Severity ratings: 0=None, 1=Slight, 2=Moderate, and 3=Pronounced visible corrosion as described in APPENDIX 2.) EXHIBIT 14 shows that moderate white rusting at several locations for pre-painted HDGA (#3) and at the dome for pre-painted HDAl (#4) . For those pre- and post-painted steels which showed slight to moderate white rusting, the white 'rust' could have been the result of reaction with the paint films. For red rusting, moderate to pronounced severities were shown by only the post-painted HDAl (#8) test material. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 23 - RESULTS AND DISCUSSION Quantitative Evaluation After 2000 Hours of Exposure The weight loss data for the test materials and the test validation coupons are shown in APPENDIXES 3 and 4 respectively. The percentage weight losses are shown graphically in EXHIBIT 15. The percentage weight losses of all specimens were very low (2% maximum) compared with the bare cold rolled steel test validation sample (12.9% loss), which indicates the effectiveness of the corrosion resistant mechanisms utilized by the various steel systems. The 2% weight loss of the post-painted HD Aluminized sample (#8) undoubtedly resulted from the loss of adhesion and blistering of the thin paint film (150µm) in all areas of the specimen (see Note 4 in APPENDIX 2). This is confirmed by the extensive creepback observed for the HD Aluminized (#8) material (see APPENDIX 5). The only severe creepback occurred in the post-painted HD Aluminized steel (#8) and was probably related to the adhesion loss of the post-paint. APPENDIX 5 also shows that no pits deeper than 0.1mm were observed in any location in any specimen. Weight loss, % (validation coupons) 60 Zinc 1500 hrs. 50 Bare CR steel 40 Weight change % (test materials) 4 30 POST-PAINTED STEELS PRE-PAINTED STEELS 2 1.1 10 Loss 0.2 0.05 -0.2 0.2 0.05 #1 #2 #3 #4 #5 #6 #7 #8 #9 304L 436L HDAl Sn-Zn HDAl 0 Gain HDGA Bare Stee l 0.7 0.3 Zn-Ni Zn Zn-Ni 0 2 0.6 Terne 1500 hrs. 2000 hrs. 304L 20 BARE STEELS #10 -2 EXHIBIT 15. Percentage weight losses (gains) of test validation samples (left) and steel test specimens (right) in the Neutral Salt Spray Test after 2000 hours exposure. The detailed gravelometer chip rating number (denoting the number of chips) and the rating letter (denoting size of the chips) and loss of adhesion for the steel system specimens after 500, 1000, 1500, and 2000 hours exposure are shown in APPENDIX 6. The results for 2000 hours exposure are summarized in EXHIBIT 16. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 24 - RESULTS AND DISCUSSION Chip frequency rating Size rating & size range of chips Rating numbers 0 1 2 3 4 5 6 7 8 9 10 A B C D Number of chips >250 150250 100159 7599 5074 2549 1024 5-9 2-4 1 0 <1mm 1-3 mm 3-6 mm >6 mm Pre-painted steels #1 EG Zn-Ni+Cr6 #2 EG Zn-Ni- Cr6 #3 HDGA- Cr6 #4 HDAℓ+ Cr6 #5 304L+Neukote Post-painted steels #6 HD Terne #7 HD Tin-Zinc #8 HDAℓ #9 Ferritic436L Bare steel #10 Austenitic 304L 1 X X X X X 1 X 1 X 1 X X No rating due to excessive blistering X2 X X X X 1 denotes loss of adhesion from metallic coating to topcoat 2 denotes loss of adhesion from steel to topcoat. EXHIBIT 16. Summary of gravelometer chip ratings after 2000 hours exposure in the Neutral Salt Spray test. The best chipping resistance was shown by those post-painted steels that had very heavy coatings (#6 & #7) and by the Austenitic 304L steel with inorganic pre-paint (#5). External - Cyclic Corrosion Test (SAE J2334) Qualitative Evaluations Photographs of all test materials after 160 cycles exposure prior to cleaning are shown in EXHIBIT 17. Additional photographs of cyclic corrosion test specimens are shown in Photo Library-Cyclic Test, identification codes for which are shown in Photo Library - LISTING 2 at the end of this report. Visual ratings of the severity of white and red rust at eight different locations for duplicate specimens are shown in APPENDIXES 7, 8 and 9 after exposure times of 80, 120 and 160 cycles, respectively. (Rust staining was not included in the ratings.) The numerical corrosion severity ratings of 0, 1, 2, and 3, are charted in EXHIBITS 18 and 19 for 120 cycle and 160 cycle exposures. The displays show moderate to pronounced white rusting only at the dome location of pre-painted HDGA (#3) and the flange area of post-painted HDAl (#8). For red rusting, moderate to pronounced severities occurred after 120 and 160 cycles at the weld clip for pre-painted Zn-Ni (#1), the scribe for pre-painted HDGA (#3), and the weld and flange for the postpainted HDAl. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 25 - RESULTS AND DISCUSSION Pre-painted steels #1 #2 #3 #5 Post-painted steels #4 #6 #7 #8 #9 Bare steel #10 EXHIBIT 17. Photographs of test materials after 160 cycles exposure and before cleaning in the Cyclic Corrosion test. (No photograph for before cleaning was available for #3. Hence, the photograph for after cleaning is shown.) Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 26 - RESULTS AND DISCUSSION EXHIBIT 18. Average corrosion severity display from the visual ratings of white and red rust after 120 cycles of exposure in the Cyclic Corrosion test. (Numeric corrosion severity ratings: 0=None, 1=Slight, 2=Moderate, and 3=Pronounced visible corrosion shown in APPENDIX 8.) Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 27 - RESULTS AND DISCUSSION EXHIBIT 19. Average corrosion severity display from the visual ratings of white and red rust after 160 cycles of exposure in the Cyclic Corrosion test. (Numeric corrosion severity ratings: 0=None, 1=Slight, 2= Moderate, and 3= Pronounced visible corrosion shown in APPENDIX 9.) Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 28 - RESULTS AND DISCUSSION Quantitative Evaluations The detailed weight changes after 80 cycles, 120 cycles and 160 cycles exposure in the Cyclic Corrosion test are shown in APPENDIXES 10, 11 and 12, respectively. To facilitate a comparison of the different steel test materials, the weight change data after 160 cycles exposure has been plotted in EXHIBIT 20. The greatest loss (2.42%) was shown by the post-painted ferritic 436L (#9) and can be attributed to the loss of the thin paint coating because no evidence of substrate corrosion was observed. Weight loss, % (average for bare cold rolled steel controls), after 80 cycles 100 80 Bare cold rolled steel control (80 Cycles) 76.0 Weight change, % (test materials) – after 160 cycles 60 4 40 Pre-painted steels Post-painted steels 2.42 Bare steel 2 20 0.55 #3 #4 #5 #6 #8 #9 #7 304L -0.57 436L #2 -0.33 -0.12 HDAl #1 Zn-Ni Gain -0.15 Sn-Zn -0.12 Terne -0.3 304L 0.09 0 Zn-Ni Bare Steel HDAl 0 0 HDGA Loss #10 -2 EXHIBIT 20. Average weight loss of cold rolled controls after 80 cycles and weight changes of steel test materials after 160 cycles exposure in the Cyclic Corrosion Test. In those instances where weight losses occurred, the percentage weight loss was very small (2.42% maximum) especially when these data are compared with the high weight loss (76%) shown by the bare cold rolled steel control after only 80 cycles, at which point the remnants of the samples were removed from the Cyclic Corrosion test cabinet. The substantial weight loss of the bare cold rolled controls confirms the severity of the Cyclic Corrosion test and the good resistance of the test materials chosen for this study. (The detailed weight loss data for the cold rolled steel control specimens are shown in APPENDIX 13.) Average creepback and average maximum pit depths for 80 cycles, 120 cycles and 160 cycles exposure to the Cyclic Corrosion test are summarized in EXHIBIT 21. (The detailed measurements are shown in APPENDIXES 14, 15 and 16.) Moderate to pronounced creepback occurred in only two postpainted test materials (HDAl #8 and Ferritic 436L #9) due to adhesion loss of the post-paint film. After 80 and 120 cycles of exposure, maximum pit depths of 0.1 and 0.2mm were observed for the two prepainted EG Zn-Ni materials (#1 & #2) and 0.4 mm for pre-painted HDAl (#4). Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 29 - RESULTS AND DISCUSSION Number of Cyclic Corrosion test cycles 80 120 160 80 120 160 Pre-painted steels #1 EG Zn-Ni + Cr6 #2 EG Zn-Ni - Cr6 #3 HDGA - Cr6 #4 HDAℓ + Cr6 #5 304L + Neukote Post-painted steels #6 HD Terne #7 HD Tin-Zinc #8 HDAℓ #9 436L Bare steel #10 304L Creepback from scribe mm Maximum pit depth /mm 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0.2* 0.1* 0 0 0 0.4* 0.4* 0 0 0 0 0 0 0 0 0 0.6 6.9 0 0 0.1 NR 0 0 0.5 2.5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 NR = no rating due to pronounced adhesion loss * = max. pit depth occurred in the gravel area EXHIBIT 21. Average creepback and average maximum pit depths after 80, 120 and 160 cycles exposure in the Cyclic Corrosion test. The pitting results for all materials are shown graphically in EXHIBIT 22 (A-C). All of the pits were observed at the gravel area and the variance associated with gravel impact probably accounts for the fact that no pits were observed after 160 cycles. It is important to understand that separate sets of specimens were used for the 80, 120 and 160 cycle specimens, it is not necessary to expect their occurence in the 160-cycle set of specimens. The origination of the pits was likely more dependent on the nature of the gravel impact than on exposure in the Cyclic Corrosion Test. EXHIBIT 22(A). Pit depths for the 80-cycle exposure set of specimens in the Cyclic Corrosion Test. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 30 - RESULTS AND DISCUSSION EXHIBIT 22(B). Pit depths for the 120-cycle exposure set of specimens in the Cyclic Corrosion Test. EXHIBIT 22(C). Pit depths for the 160-cycle exposure set of specimens in the Cyclic Corrosion Test. The detailed gravelometer chip ratings are shown in APPENDIXES 17, 18 and 19. A summary of data after 160 cycles is shown in EXHIBIT 23. The pre-painted steels, in general, had 10 - 74 chips that were less than 1 mm in size. For the post-painted steels, a higher frequency (50 - 159) of chips of larger size (3 - 6 mm) were observed for the HDAl (#8) and Ferritic the 436L (#9) steels, which resulted from the paint adhesion loss. By comparing the 160 exposure data Ferritic (EXHIBIT 23) with data from 20 cycle exposure (see EXHIBIT 24), it can be seen that there is little change in chip rating and size for the prepainted steels. This indicates that the gravel impact determines the chip ratings more than the corrosion exposure cycles. However, for the post-painted materials (#8 & #9), the chip frequency increased somewhat as the corrosion exposure (and number of gravel impacts) increased. Chip frequency rating Size rating & size range of chips Rating numbers 0 1 2 3 4 5 6 7 8 9 10 A B C D Number of chips >250 150250 100159 7599 5074 2549 1024 5-9 2-4 1 0 <1 mm 1-3 mm 3-6 mm >6 mm X X X X X X X X — — — — — — X X — — X — — — — Pre-painted steels 6 #1 EGZn-Ni+Cr #2 EGZn-Ni-Cr6 6 #3 HDGA-Cr 6 #4 HDAℓ+Cr #5 304L+Neukote #6 HD Terne #7 HD Tin-Zinc #8 HDAℓ #9 436L 1 X1 X1 X 2 X Post-painted steels 1 X X2 1 X2 X Bare Steel #10 304L 1 denotes adhesion loss between metallic coating and topcoat 2 denotes adhesion loss between steel and topcoat EXHIBIT 23. Summary of gravelometer chip ratings after 160 cycle exposure in Cyclic Corrosion Testing. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 31 - RESULTS AND DISCUSSION Chip frequency Size rating & size range of chips Rating numbers 0 1 2 3 4 5 6 7 8 9 10 A B C D Number of chips >250 150250 100159 7599 5074 2549 1024 5-9 2-4 1 0 <1 mm 1-3 mm 3-6 mm >6 mm — — — — — — — — — — — 6 Pre-painted steels #1 EGZn-Ni+Cr 6 #2 EGZn-Ni-Cr 6 #3 HDGA-Cr 1 X 1 X X X X 1 X 6 1 #4 HADℓ+Cr #5 304L+Neukote X X — X Post-painted steels #6 HD Terne #7 HD Tin-Zinc #8 HADℓ #9 436L X X 1 X — — X 2 X X Bare Steel #10 304L X — — 1 denotes adhesion loss between metallic coating and topcoat 2 denotes adhesion loss between steel and topcoat EXHIBIT 24. Summary of gravelometer chip ratings after 20 cycles of exposure in the Cyclic Corrosion Testing (from the set of specimens used for the 160-cycle evaluations shown in EXHIBIT 23). Internal Fuel Test The steel systems tested in the fuel test are re-listed in EXHIBIT 25 to show the type of surface exposed to the fuels. (A more detailed description of the steels and surfaces has already been given in EXHIBIT 11). Steel ID Number Bare Steel Metallic Coating Surface Exposed to the Test Fuel Pre-painted category of steels 1 Low carbon steel EG Zn-Ni Metallic coating + Magni pre-paint (with Cr+6) 2 Low carbon steel EG Zn-Ni Metallic coating + Magni pre-paint +6 (without Cr ) 3 Low carbon steel Hot dip galvannealed Metallic coating + Magni pre-paint +6 (without Cr ) 4 Low carbon steel Hot dip aluminized Metallic coating + Magni pre-paint (with Cr ) 5 Austenitic stainless None Steel + Neukote inorganic coating +6 Post-painted category of steels 2 6 Low carbon steel Hot dip terne Metallic coating + Phosphate (3mg/m ) 7 Low carbon steel Hot dip Tin-Zinc Metallic coating + Cr-free resin (300mg/ m ) 8 Low carbon steel Hot dip Aluminized Metallic coating + Chromate 9 Ferritic stainless steel None Bare steel None Bare steel 2 Bare steels category 10 Austenitic stainless EXHIBIT 25. Summary of steels used for fuel resistance testing showing the nature of the surface exposed to the test fuel. (For details of the metallic coatings and exterior surface paints, see EXHIBIT 11.) Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 32 - RESULTS AND DISCUSSION Qualitative Evaluations The photographs of initial fuel test specimens after 28 weeks and 39 weeks exposure are shown in the attached file Photo Library for Fuel Test, for which identity codes are shown in Photo Library – LISTING 3. The detailed visual observations are shown in APPENDIXES 20 to 29. Except for one pin-point red rust spot on the lid of one specimen (pre-painted EG Zn-Ni #1) after 20 weeks, the only surface change observed was the appearance of a white residue. It was unclear whether the white residue represented corrosion of the steel or a reaction product with the fuel. The extent of the white residue was recorded according to the same rating scale used in visually rating the external corrosion test specimens. The numerical visual ratings are shown in EXHIBITS 26, 27 and 28. EXHIBIT 26. Extent of white residue at the fuel-contact area of the test cups. (Numeric ratings: 0=None, 1=Slight, 2=Moderate, and 3=Pronounced visible residue shown in APPENDIXES 20-29.) For the fuel-contact area, only one material (Terne, #6) showed moderate to pronounced white residue after 39 weeks. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 33 - RESULTS AND DISCUSSION EXHIBIT 27. Extent of white residue at the fuel-vapor interface area of the test cups. (Numeric ratings: 0=None, 1=Slight, 2=Moderate, and 3=Pronounced visible corrosion shown in APPENDIXES 20-29.) In general, the extent of white residue was more severe at the fuel-vapor interface area, EXHIBIT 27. At this location, although there was zero residue for the four pre-painted materials (#1-#4) after all exposures, moderate to pronounced residue was observed for all other materials starting at 28 weeks of exposure. This might be expected in view of the minimal coating or absence of coatings in the latter materials. EXHIBIT 28. Extent of white residue at the vapor area of the test cups. (Numeric ratings: 0=None, 1=Slight, 2=Moderate, and 3=Pronounced visible residue shown in APPENDIXES 20-29.) Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 34 - RESULTS AND DISCUSSION At the vapor-contact area, only moderate residues were observed for one material (Terne, #6) after 32 weeks of exposure. It should be emphasized that, although the moderate and pronounced ratings refer to the area affected, the depth or thickness of the white residue was so small that no scrapings could be taken to conduct an analysis of the residue. Quantitative Evaluation for Fuel Test The weight changes for the fuel test cups and lids are summarized in EXHIBITS 29 and 30 respectively, after the full 39 weeks exposure. (The detailed actual weights and progressive weight losses from 0 to 39 weeks for cups and lids are shown in APPENDIXES 30 to 33). CUPS: Initial (g) Final (g) Change (g) % Weight loss (Gain) Actual Rounded Pre-painted steels 1. EG Zn-Ni 6 +Cr 2. EG Zn-Ni 6 Cr 6 3. HDGA - Cr 6 4. HDAℓ + Cr 5. 304L Stainless + Neukote 58.7196 59.5354 59.1027 61.1080 61.2032 60.2463 50.1409 50.8337 50.6874 56.1806 56.2672 56.1086 69.8092 69.7561 69.4543 58.7143 59.5312 59.0974 61.1033 61.1976 60.2422 50.0802 50.7798 50.6291 56.1725 56.2588 56.0961 69.8172 69.7608 69.4563 -0.0053 -0.0042 -0.0053 -0.0047 -0.0056 -0.0041 -0.0607 -0.0539 -0.0583 -0.0081 -0.0084 -0.0125 0.0080 0.0047 0.0020 -0.0090 -0.0071 -0.0090 -0.0077 -0.0068 -0.0068 -0.1211 -0.1060 -0.1150 -0.0144 -0.0149 -0.0223 0.0115 0.0067 0.0029 0.01 0.01 0.01 0.01 0.01 0.01 0.12 0.11 0.12 0.01 0.01 0.02 0.01 0.01 0 51.1515 51.1739 51.1658 51.3344 51.3981 51.3340 54.6739 54.7048 54.5910 50.8958 50.8646 50.7450 51.1299 51.1572 51.1552 51.3294 51.3946 51.3303 54.6732 54.7047 54.5829 50.8956 50.8663 50.7481 -0.0216 -0.0167 -0.0106 -0.0050 -0.0035 -0.0037 -0.0007 -0.0001 -0.0081 -0.0002 0.0017 0.0031 -0.0422 -0.0326 -0.0207 -0.0097 -0.0068 -0.0072 -0.0013 -0.0002 -0.0148 -0.0004 0.0033 0.0061 0.04 0.03 0.02 0.01 0.01 0.01 0 0 0.01 0 0 (0.01) 69.0016 69.0689 69.1909 69.0003 69.0702 69.1894 -0.0013 0.0013 -0.0015 -0.0019 0.0019 -0.0022 0 0 0 Post-painted steels 6. HD Terne 7. HD Tin-Zinc 8. HDAℓ 9. Ferritic Stainless Bare Steel 10. 304L Stainless * No painted surface in contact with fuel. EXHIBIT 29. Weight changes for the fuel test cups after the maximum exposure to the fuel of 39 weeks. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 35 - RESULTS AND DISCUSSION LIDS: Initial (g) Final (g) Change (g) % Weight Loss Actual Rounded Pre-painted 1. EG Zn-Ni 6 +Cr 2. EG Zn-Ni 6 Cr 6 3. HDGA - Cr 6 4. HDA? + Cr 5. 304L Stainless + Neukote 33.5038 33.5193 33.4456 34.4235 34.3345 34.1355 28.531 29.1547 29.2427 31.793 31.7794 31.7456 39.4244 39.4167 39.3869 33.4993 33.5149 33.4413 34.4089 34.3234 34.1257 28.4939 29.1163 29.2038 31.7728 31.7592 31.7225 39.4241 39.4166 39.3869 -0.0045 -0.0044 -0.0043 -0.0146 -0.0111 -0.0098 -0.0371 -0.0384 -0.0389 -0.0202 -0.0202 -0.0231 -0.0003 -0.0001 0.0000 -0.0134 -0.0131 -0.0129 -0.0424 -0.0323 -0.0287 -0.1300 -0.1317 -0.1330 -0.0635 -0.0636 -0.0728 -0.0008 -0.0003 0.0000 0.01 0.01 0.01 0.04 0.03 0.03 0.13 0.13 0.13 0.06 0.06 0.07 0 0 0 28.9321 29.0172 28.9316 30.8197 30.7312 30.7848 28.5956 28.6851 28.6737 28.7993 28.7165 28.8122 28.9327 29.0174 28.9318 30.8178 30.7313 30.7848 28.5961 28.6863 28.6740 28.7958 28.7125 28.8081 +0.0006 +0.0002 +0.0002 -0.0019 +0.0001 0 +0.0005 +0.0012 +0.0003 -0.0035 -0.0040 -0.0041 +0.0021 +0.0007 +0.0007 -0.0006 +0.0003 0 +0.0017 +0.0042 +0.0010 -0.0122 -0.0139 -0.0142 0 0 0 +0.01 39.079 38.9524 39.0745 39.0784 38.952 39.0738 -0.0006 -0.0004 -0.0007 -0.0015 -0.0010 -0.0018 0 0 0 Post-painted 6. HD Terne 7. HD Tin-Zinc 8. HDA? 9. Ferritic Stainless 0 0 0 0 0 0 0 Bare Steels * No painted surface in contact with fuel. EXHIBIT 30. Weight changes for the fuel test lids after the maximum exposure to the fuel vapor of 39 weeks. The weight changes for both cups and lids were extremely small - in general, less than 0.01 percent although for the pre-painted HDGA (#3), weight losses were 0.12 and 0.13 percent for the cups and lids, respectively. The very low weight losses confirm the very slight corrosion observed by visual inspection. No pits were observed in any material after any exposure. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 36 - SUMMARY OF RESULTS The results of external corrosion testing are reviewed in relation to the two specific tests which were conducted, as follows: Neutral Salt Spray Test Results The results obtained from qualitative and quantitative evaluations indicated that the corrosion was variable across different regions of the specimens and was not severe enough to cause perforation (failure). In fact, no pits deeper than 0.1mm were observed for any materials. The complete results are best reviewed by category of the steel systems. Pre-Painted Steels For the most part, the steels showed only slight or no corrosion. However, there was modest white rust at the dome, scribe and chip area of pre-painted HDGA #3 after 2000 hours of exposure. The weight losses for all the pre-painted steels were low (0.17 to 1.12%) compared with the bare steel test validation sample (12.9 to 13%). Despite the fact that there was some paint chipping for all prepainted samples, (except the inorganic coated stainless (#5)), which exposed the metallic coating, no corrosion pits deeper than 0.1mm were found. None of the pre-painted samples showed any creepback at the scribe line. Post-Painted Steels Although all of these steels performed satisfactorily in that no perforation occurred (in fact, no pits deeper than 0.1mm were observed), the relative performance depended on the efficiency of the paint coatings. For example: - the thick paints (350-370µm) of the HD Terne and HD Tin-Zinc steels (#6 and #7) showed excellent resistance to chipping, almost no visible corrosion, very low weight losses (.01 to 0.04%) and no creepback. - the HD Aluminized steel (#8) showed severe loss of adhesion of the thin paint film (150µm) after gravel impact and 1500 and 2000 hours exposure. As a result, some pronounced red rusting (as shown in EXHIBIT 31) occurred at the dome, chip and field areas and extensive creepback was observed. Despite this, the base material showed only 2% weight loss and no pits deeper than 0.1mm. - the 436L stainless steel (#9) showed extensive adhesion loss of the thin (20µm) paint after gravel impact, but no creepback at the scribe line, only a small overall weight loss (0.7%) and no pits deeper than 0.1mm. Bare Steel The bare 304L steel showed some local red rusting, but a low weight loss (0.33% after 2000 hours exposure). The visual ratings and photographs showed that most of the corrosion occurred on the flange (top and bottom) near the weld and the gravel area (EXHIBIT 32). However, no pits deeper than 0.1mm were observed even at the weld area, thus, satisfactory performance was shown even after 2000 hours exposure. All results for the above steel categories are summarized in tabular form in EXHIBIT 33. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 37 - SUMMARY OF RESULTS EXHIBIT 31. Moderate to pronounced red and white rusting of HDAl (#8) post-painted with thin paint film - (Photo ID #092000nss aft) after 2000 hours Neutral Salt Spray exposure. PRE-PAINTED STEELS Visual Evaluation In general, only slight or no corrosion • Modest white rust at dome, scribe and chip area of HDGA #3 Weight loss Low losses • Max. loss (1.1%) for HDAl #4 EXHIBIT 32. Local red rusting in the 304L stainless steel #10 after 2000 hours of Neutral Salt Spray Exposure (Photo ID #102000nss aft) after 2000 hours Neutral Salt Spray exposure. POST-PAINTED STEELS BARE STEEL Corrosion and paint adhesion depended on paint film thickness. • For materials with thick paints (HD Terne #6 and HD Tin-Zinc #7) no visible corrosion and excellent chip resistance. • For materials with thin paints (HDAl #8 & 436L #9) showed severe paint loss, modest to pronounced rust for HDAl #8 but no rust for 436L #9. Local red rusting for 304L • flange near weld • gravel area Low losses • Max. weight losses for 436L #9 (0.7%) and HDAl #8 (2.0%) likely related to paint loss. Low loss (0.2%) for 304L All steel categories showed low losses compared with 3% for bare carbon steel. Creepback at scribe None Severe for HDAl #8 Pit depth (deeper than 1mm) None None Chip rating in gravel area Moderate chipping (10-49 chips, less than 1mm) and down to the metallic coating for epoxy prepaints (#1 to #4). No chipping of the inorganic coated 304L #5 steel. —— None No chipping for thick-paint samples (HD Terne #6 & HD TinZinc #7) Moderate chipping & 1-3mm chip size for 436L #9 Severe blistering of HDAl #8 —— EXHIBIT 33. Summary of NEUTRAL SALT SPRAY TEST results (after 2000 hours exposure). Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 38 - SUMMARY OF RESULTS Cyclic Corrosion Test Results As with the Neutral Salt Spray results, the Cyclic Corrosion test results showed that corrosion was variable across the different regions of the individual specimens and not serious enough to cause failure (perforation). Of interest is the comparison of weight losses for bare steel control coupons after exposure in the the Cyclic test (after 80 cycles) and in the Neutral Salt Spray test (2000 hours). The former showed a loss of 76%, whereas, the later was 12.9%. This indicates the greater corrosion severity of the Cyclic test. For the test materials, it was difficult to see definitive trends in any of the weight change data (EXHIBIT 20) because in many cases there were gains (up to 2.49% for the bare Austenitic 304L steel) and losses (up to 2.42% for the Ferritic 436L steel, which was likely due to paint loss and not due to steel corrosion). The fact that these changes were small compared with a reference weight loss of 76% for bare steel after only 80 cycles, indicates that very little steel corrosion weight loss occurred for all test materials. The significance of the results is best discussed by the category of steel systems. Pre-Painted Steels The visual ratings of corrosion (EXHIBITS 18 and 19) for the most part showed either none, slight or moderate corrosion for most locations of the pre-painted materials. However, the EG Zn-Ni #1 material showed moderate to pronounced red rust at the weld area after 160 cycles (see EXHIBIT 34). All materials showed zero creepback at the scribe line, but some pits were observed after 80 and 120 cycles for the EG Zn-Ni + Cr6 (#1) and the HD Aluminized steels. However, the pits in the gravel impact area were well below the perforation level. The fact that some materials showed no pits after 160 cycles exposure indicates that pitting may have been more dependent on the variability of the gravel impact than on the length of cyclic corrosion exposure. The gravelometer results showed some paint chipping for all pre-painted samples, but the frequency of the chips was moderate (10 - 49) and the size of chips was, in general, low (<1mm to 3mm). For the epoxy pre-painted materials (#1-#4), the chipping occurred early (after 20 cycles) but did not change significantly after longer cycle exposures. EXHIBIT 34. Moderate to pronounced red rusting at the weld area of pre-painted EG Zn-Ni #1 after 160 cycles in the Cyclic Corrosion Test (Photo ID #01 J2334-160bef.2) Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 39 - SUMMARY OF RESULTS Post-Painted Steels Those materials having thick post-paint films, i.e., HD Terne (#6), HD Tin-Zinc (#7) had no visual corrosion at any location for all exposures. The thinner paint coating (150µm) on the HD Aluminized steel (#8) had red rusting at the flange and weld after 160 cycles (see EXHIBIT 35) but almost no rusting at other areas. For the Ferritic 436L material, no corrosion was observed despite a pronounced adhesion loss of the zinc-rich paint. The extent of creepback at the scribe line generally paralleled the visual observations - no creepback for the heavily painted materials (#6 and #7), small amounts for the HD Aluminized (#8) and significant amounts for the Ferritic 436L (#9), which had substantial paint adhesion loss. The variations in paint adhesion performance accounted for the difference in the gravelometer chip ratings: - no chips for the HD Terne and HD Tin-Zinc materials (up to 370µm thick paint films) - some chipping for the HD Aluminized steel (150µm paint) - extensive chipping for the Ferritic 436L steel (20µm paint) No pits (deeper than 0.1mm) were observed for any post-painted material at any location for exposures through 160 cycles. Bare Steel For the most part, very minor visual ratings of corrosion (none to slight) were shown by the Austenitic 304L (#10) for exposures through 160 cycles. Some moderate red rusting was observed at the weld area after 160 cycles (see EXHIBIT 36). The Cyclic Corrosion Test results are summarized in EXHIBIT 37. EXHIBIT 35. Moderate to pronounced red rusting at the flange and weld area of thin (150µm) post-painted HDAl #8 steel after 160 cycles in the Cyclic Corrosion Test. (Photo ID #09 J2334-160bef.2) EXHIBIT 36. Localized red rusting at the weld of the 304L stainless steel (#10) after 160 cycles in the Cyclic Corrosion Test. (Photo ID #10 J2334-160bef.2) Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 40 - SUMMARY OF RESULTS PRE-PAINTED STEELS Visual Evaluation In general, none to moderate corrosion observed • Moderate to pronounced red rust occurred at weld for EG Zn-Ni #1 and at scribe for EG Zn-Ni #2 Weight loss Very low weight losses (0 – 0.55%) POST-PAINTED STEELS BARE STEEL Corrosion performance varied according to thickness and adhesion of paint films • None to slight red rust (scribe) for thick paints (HD Terne #6 & HD Tin-Zinc #7) • Moderate to pronounced red rust at flange & weld for thinpaint HDAl#8 • No rust for 436L #9 None to slight variable red rust in most locations and moderate rust at weld for 304L #10 Max. weight loss (2.42%) shown by 436L #9, but probably due to paint loss No weight loss The weight losses of all materials after 160 cycles was very low compared with 76% loss for bare carbon steel after only 80 cycles exposure. Creepback at scribe None Pit depth (deeper than 0.1mm) 0.1 to 0.2mm single pits observed in gravel area of EG Zn-Ni #1 & #2 (after 80 & 120 cycles) 0.4mm single pits observed in gravel area of HDAl #4 (after 80 & 120 cycles) No pits observed for 160 cycle exposure specimens. Chip rating in gravel area Moderate chipping (10-49 chips, less than 1mm) and down to metallic coating for epoxy pre-painted steels (#1 to #4). Moderate chipping (10-74 chips, <1mm to 3mm) for inorganic painted 304L #5. —— None for materials having thick paint films (HD Terne #6 & HD Sn-Zn #7) Moderate to severe for thin paint films (HDAl #8 * 436L #9) None None No chipping for HD Terne #6 & HD Tin-Zinc #7 Moderate chipping (50-74 chips, 36mm) for HDAl #8 Severe chipping (100-159 chips, 36mm) for 436L #9 —— * The un-painted surface was in contact with the fuel (See EXHIBIT 25) EXHIBIT 37. Summary of CYCLIC CORROSION TEST results (after 160 cycles exposure). Internal (Fuel) Corrosion Test Results The visual ratings of cups and lids (shown in EXHIBITS 26-28) showed pronounced white residue only at the fuel- vapor interface for the post-painted and bare steel categories. For all steels in these categories, the fuel and vapor impinged on either a treated metallic coating or the bare steel surfaces (430L Ferritic stainless #9 and 340L Austenitic stainless #10). As a consequence, a ring of attack occurred at the fuelvapor interface - in some cases it appeared as an 'etched' surface and in others a 'film-like' deposit. For the pre-painted materials where the pre-paint was in contact with the fuel and vapor, no ring or concentrated attack was observed at the fuel-vapor interface. Either visual ratings of 'none,' 'slight' or 'moderate' were observed for all specimens that contacted either the fuel (base of cups) or vapor (cup walls and lids). The very small weight losses (less than 0.12% for cups and 0.13% for lids) after 39 weeks of exposure confirm that only minor corrosion, cosmetic in nature, took place. A photograph of the pre-painted HDGA #3 which had the largest weight loss (0.12 to 0.13%) is shown in EXHIBIT 38. In fact, where some corrosion products were observed, they were so slight that no scrapings could be procured for a chemical analysis. No pits (deeper than 0.1mm depth) were observed in any of the materials. The results of the Internal (Fuel) Corrosion tests are summarized in EXHIBIT 39. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 41 - SUMMARY OF RESULTS EXHIBIT 38. Fuel cups and lids of pre-painted HDGA #3 after 39 weeks exposure to aggressive CE10A fuel. PRE-PAINTED STEELS POST-PAINTED STEELS BARE STEEL Visual Evaluation For all materials, there was no evidence of ‘corrosion’ except a white residue was observed to varying extents, but largely at the fuel-vapor interface. (The extent of the residue was insufficient to conduct an analysis.) No white residue in fuel and interface areas. Slight residue in vapor area Slight to moderate white residue in fuel and vapor areas. Pronounced residue at fuel-vapor interface. No residue in fuel and vapor areas. Pronounced residue at fuel-vapor interface for 304L #10. Weight loss Very minor losses generally for cups & lids • Max. weight loss of 0.13%) for HDAGl #3 Very minor weight losses generally for cups and lids • Max. weight loss of <0.04% for HD Terne #6 No weight loss. Pit depths (deeper than 0.1mm) None None None ** The un-paid surface was in contact with the fuel (See EXHIBIT 25) EXHIBIT 39. Summary of INTERNAL (FUEL) CORROSION TEST results (after 39 weeks exposure). Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 42 - CONCLUSIONS Simulative External Corrosion Testing, by Neutral Salt Spray and Cyclic Corrosion tests, of 10 different steel systems has shown that: - No perforation (failure) was observed, either after 2000 hours Salt Spray exposure or 160 cycles of Cyclic exposure (simulating 20 years of fuel tank life), in any of the steel systems. - The extent of corrosion varied according to the location on the specimen (dome, scribe line, weld, and gravel impact area) and from steel to steel. However, these variations did not threaten perforation (failure) in any of the systems. (The maximum pit depths were 20 to 40% of steel thickness.) Furthermore, these variations were not of such significance to be able to rate one steel system over another. - The integrity of the paint systems varied according to the thickness of the paint. - Those steels (EG Zn-Ni and HD Aluminized) pre-painted with thin epoxy films (9µm) and the Austenitic 304L steel + Neukote inorganic film (17µm) showed small amounts of paint chip loss after initial gravel impacts, but did not deteriorate after additional gravel impacts and exposures. Those post-painted steels (HD Terne and HD Tin-Zinc) having thick acrylic and top coat paints (up to 370 µm) showed no paint loss by chipping or creepback at the scribe line. Those steels post-painted with thinner films (i.e., the 150µm alkyd paint on HD Aluminized steel and the 20µm zinc-rich paint on Ferritic 436L steel) had adhesion losses (after gravel impact and from creepback at the scribe line) proportional to their coating thicknesses. This suggests that the thickness of these paint films could be increased to further improve paint integrity which depends on the combination of coating and paint system. - The early withdrawal of two additional steel systems from external corrosion testing, because of inadequate paint film thicknesses, indicates the severity of the external corrosion tests employed. Simulative Internal Corrosion Testing of sealed cups assembled from the 10 steel systems and exposed to an aggressive alcohol-containing gasoline (CE10A) showed only minor corrosion even after exposures of 39 weeks (representing 15-year fuel tank life). Where some corrosion occurred, there was insufficient reaction product to enable an analysis to be conducted. No pitting (deeper than 0.1mm depth) was observed in any of the steel systems regardless of different locations in the cups which allowed either full contact with the fuel, contact at the fuel-vapor interface or full vapor contact. As a result of the above specific conclusions, it is expected that all of the special steel systems tested in this study will resist perforation corrosion (in the severe external environments experienced by automobile fuel tanks) for up to 20 years. Additionally, it is expected that all of the steel systems tested in this study will resist corrosion from an aggressive fuel such as CE10A for at least 15 years. Thus, it is fully anticipated that all of the systems will meet the 15-year durability requirements of California's Air Resources Board. All of the steel systems tested in this work are commercially available from the worldwide steel industry. The selection of one steel system over another will depend on factors beyond corrosion resistance. These may include: - the manufacturing approach favored by the automakers (i.e., use of pre-painted steels, post-painting or use of bare steels) - material and manufacturing costs - inherent formability and weldability of the steels - forming and welding equipment available The above factors are beyond the scope of this report and specific selection and application criteria should be discussed with steel suppliers. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 43 - REFERENCES AND NOTES [1] F.W. Lutze, D.C. McCune, J.R. Schaffer, K.A. Smith, L.S. Thompson, and H.E. Townsend, “Interlaboratory Testing to Evaluate improvements in the precision of the SAE J2334 Cyclic Corrosion Test,” Proceedings of the Fifth International Conference on Zinc and Zinc Alloy Coated Steel Sheet, Centre for Research in Metallurgy, Brussels, Belgium, (June 2001) [2] F.W. Lutze, D.C. McCune, H.E. Townsend, K.A. Smith, R.J. Shaffer, L.S. Thompson, and H.D. Hilton,“The Effects of Temperature and Salt Concentration on the Speed of the SAE J2334 Cyclic Corrosion Test,” Proceedings of the European Corrosion Congress, London, (2000) [3] R.J. Shaffer, “Practical Test Results Using the SAE J2334 Accelerated Corrosion Test,” Proceedings of the European Corrosion Congress, London, (2000) [4] Dennis Davidson, et al, “Perforation Corrosion Performance of Autobody Steel Sheet in On-Vehicle and Accelerated Tests,” SAE 2003-01-1238 [5] “Standard Practice for Operating Salt Spray (Fog) Apparatus,” ASTM Designation: B117-02 [6] “Cosmetic Corrosion Lab Test,” SAE J2334 (Revised October 2002) [7] “Test for Chip Resistance of Surface Coatings,” SAE J400 (Revised 2002-11) [8] “Gasoline, Alcohol and Diesel Fuel Surrogates for Materials Testing,” SAE J1681 (Rev. Jan. 2000) [9] “Recommended Methods for Conducting Corrosion Tests in Gasoline/Methanol Fuel Mixtures,” SAE &1747 (Dec. 1994) [10] “Standard Test Method for Ball Punch Deformation of Metallic Sheet Material,” ASTM Designation: E653-84 (Re-approved 2000) [11] “Standard Test Method for Evaluation of Painted or Coated Specimens Subjected to Corrosive Environments,” ASTM Designation: D1654-00 [12] For the first 4-week exposure to fuel, Viton A was used for the gasket and some slight degradation of the gasket was observed. Subsequently, for the remaining exposures (4 to 39 weeks) Viton F was used and no degradation occurred. [13] A pre-trial of 2 months (2 fuel loadings) indicated no loss of fuel after each of the 2 four-week exposures. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 44 - ACKNOWLEDGMENTS The guidance and input received from several automakers (General Motors Corporation, Ford Motor Company, DaimlerChrysler Corporation, Nissan, Toyota, FHI-Subaru, Fiat, Jaguar, and VW) concerning the corrosion tests, methodology, specimen configuration, and materials is greatly appreciated. In particular, the assistance from Martin Stephens and Trevor Enge (DaimlerChrysler), Jola Lott, Li Hussain and Jim Oldfield (Ford), Peter Nguyen (GM), and Jon Sussman (Nissan) is gratefully acknowledged. Special thanks are due to Frank Topolovec (Ford) for welding many of the External Test specimens and to James Layland and Elmer Wendell of Homer Research Laboratories, Bethlehem Steel (now International Steel Group) for forming the domes of the specimens, as well as for forming the cups and cutting the lids for the Internal Fuel Test assemblies and coordinating the supply of all samples to ACT Laboratories. Significant technical contributions, as part of early participation in the Corrosion Evaluation Team by Stavros Fountoulakis and Steve Jones of Bethlehem Steel (now International Steel Group), Bruce Hartley (then of National Steel), Laurent Dallemagne (Arcelor), Art Coleman (then of J & L Specialty Steel), and Juergen Froeber (TKS) are acknowledged and appreciated. The Corrosion Evaluation Team of SASFT is grateful to ACT Laboratories for their diligent testing and communications. In particular, Julie Piper, Frank Lutze and Kevin Wendt were of key help in conducting this program. Finally, those special experts and technicians within the steel companies who provided valuable information and guidance is greatly appreciated. Evaluation of the Corrosion Durability of Steel Systems for Automobile Fuel Tanks - 45 - LIST OF ATTACHMENTS PHOTO LIBRARY Listing 1: Neutral Salt Spray – photo identification codes Listing 2: Cyclic Corrosion – photo identification codes Listing 3: Fuel Test – photo identification codes APPENDIXES Number Description 1. Reference information supporting the value of the J2334 Cyclic Test 2. Visual ratings of rust after 2000 hours in the Neutral Salt Spray Test. 3. Weight change of steel materials after 2000 hours exposure in the Neutral Salt Spray Test. 4. Weight loss of test validation coupons in the Neutral Salt Spray Test. 5. Creepback from scribe line and maximum pit depths for steels after exposure of 2000 hours in the Neutral Salt Spray Test. 6. Gravelometer chip ratings of steel test materials after 500, 1000, 1500 and 2000 hours exposure in the Neutral Salt Spray Test. 7. Visual ratings of corrosion severity after 80 cycles in the Cyclic Corrosion Test. 8. Visual ratings of corrosion severity after 120 cycles in the Cyclic Corrosion Test. 9. Visual ratings of corrosion severity after 160 cycles in the Cyclic Corrosion Test. 10. Weight-change data for steel test materials and bare cold-rolled steel samples after 80 cycles exposure in the Cyclic Corrosion Test. 11. Weight-change data for steel test materials and bare cold-rolled steel samples after 120 cycles exposure in the Cyclic Corrosion Test. 12. Weight-change data for steel test materials and bare cold-rolled steel samples after 160 cycles exposure in the Cyclic Corrosion Test. 13. Weight loss of bare cold-rolled steel control samples after 80 cycles exposure In the Cyclic Corrosion Test. 14. Creepback and maximum pit depths for steel test materials after 80 cycles exposure in the Cyclic Corrosion Test. 15. Creepback and maximum pit depths for steel test materials after 120 cycles exposure in the Cyclic Corrosion Test. 16. Creepback and maximum pit depths for steel test materials after 160 cycles exposure in the Cyclic Corrosion Test. 46 17. Gravelometer chip ratings for the 80-cycle exposure set of steel test materials. 18. Gravelometer chip ratings for the 120-cycle exposure set of steel test materials. 19. Gravelometer chip ratings for the 160-cycle exposure set of steel test materials. 20. Extent of corrosion (white residue) and observations after 4 weeks in the Fuel Test. 21. Extent of corrosion (white residue) and observations after 8 weeks in the Fuel Test. 22. Extent of corrosion (white residue) and observations after 12 weeks in the Fuel Test. 23. Extent of corrosion (white residue) and observations after 16 weeks in the Fuel Test. 24. Extent of corrosion (white residue) and observations after 20 weeks in the Fuel Test. 25. Extent of corrosion (white residue) and observations after 24 weeks in the Fuel Test. 26. Extent of corrosion (white residue) and observations after 28 weeks in the Fuel Test. 27. Extent of corrosion (white residue) and observations after 32 weeks in the Fuel Test. 28. Extent of corrosion (white residue) and observations after 36 weeks in the Fuel Test. 29. Extent of corrosion (white residue) and observations after 39 weeks in the Fuel Test. 30. Actual weights of fuel test cups after 0 to 39 weeks exposure in the Fuel Test. 31. Weight changes of fuel test cups after 4 to 39 weeks exposure in the Fuel Test. 32. Actual weights of lids after 0 to 39 weeks exposure in the Fuel Test. 33. Weight changes of lids after 4 to 39 weeks exposure in the Fuel Test. 47 PHOTO LIBRARY – LISTING 1 Neutral Salt Spray Test Specimens. (for photos see file: Photo Library-Neutral Salt Spray) 1-A ID# Material Pre-painted steels Photo Code 1 EG Zinc-Nickel (with Cr6) 2 EG Zinc-Nickel (no Cr6) 3 HDGA (Zn-Fe) (no Cr6) 4 HD Aluminized (no Cr6) 5 Austenitic 304L with Neukote #01 NSSi #01 1000 NSS I #01 1000 NSS F #01 2000 NSS BEFORE #01 2000 NSS AFTER #02 NSS i #02 1000 NSS I #02 1000 NSS F #02 2000 NSS BEFORE #02 2000 nss aft #03 NSSi #03 1000 NSS i #03 1000 NSS F #03 2000 hr. NSS bef #03 2000 hr. NSS aft #04 NSSi #04 1000 NSS I #04 1000 NSS F #04 2000 NSS BEFORE #04 2000 nss aft #11 NSSi #11 1000 NSS I #11 1000 NSS F #11 2000 NSS BEFORE #11 2000 nss aft Exposure (hrs) 0 1000 1000 2000 2000 0 1000 1000 2000 2000 0 1000 1000 2000 2000 0 1000 1000 2000 2000 0 1000 1000 2000 2000 Condition After gravel Before gravel After gravel Before cleaning After cleaning After gravel Before gravel After gravel Before cleaning After cleaning After gravel Before gravel After gravel Before cleaning After cleaning After gravel Before gravel After gravel Before cleaning After cleaning After gravel Before gravel After gravel Before cleaning After cleaning PHOTO LIBRARY – LISTING 1 48 PHOTO LIBRARY – LISTING 1 (continued) Neutral Salt Spray Test Specimens. (for photos see file: Photo Library-Neutral Salt Spray) 1-B ID# in Report Post-painted steels Material 6 HD Terne 7 HD Tin-Zinc 8 HD Aluminized 9 Ferritic 436L Stainless Photo ID Code #05 NSSi #05 1000 NSS I #05 1000 NSS F #05 2000 NSS BEFORE #05 2000 nss aft #06 NSSi #06 1000 NSS I #06 1000 NSS F #06 2000 NSS BEFORE #06 2000 nss aft #09 NSSi #09 1000 NSS I #09 1000 NSS F #09 2000 NSS BEFORE #09 2000 nss aft #13 NSSi #13 1000 NSS I #13 1000 NSS F #13 2000 NSS BEFORE #13 2000 nss aft 1-C ID# in Report 10 Material Austenitic 304L Stainless Exposure (hrs) 0 1000 1000 2000 2000 0 1000 1000 2000 2000 0 1000 1000 2000 2000 0 1000 1000 2000 2000 Condition After gravel Before gravel After gravel Before cleaning After cleaning After gravel Before gravel After gravel Before cleaning After cleaning After gravel Before gravel After gravel Before cleaning After cleaning After gravel Before gravel After gravel Before cleaning After cleaning Bare steels Photo ID Code #10 NSSi #10 1000 NSS I #10 1000 NSS F #10 2000 NSS BEFORE #10 2000 nss aft Exposure (hrs) 0 1000 1000 2000 2000 Condition After gravel Before gravel After gravel Before cleaning After cleaning PHOTO LIBRARY – LISTING 1 (continued) 49 PHOTO LIBRARY – LISTING 2 Cyclic Corrosion Test Specimens. (for photos see file: Photo Library-Cyclic Test) 2-A ID# in Report 1 2 3 Test Material EG ZincNickel + Cr6 EG ZincNickel - Cr6 HDGA (ZnFe) - Cr6 Pre-painted steels Photo ID Code #01 J2334-160i Exposure, cycles 0 Condition After gravel #01 J2334-120 bef #01 J2334-120 bef-2 120 120 #01 J2334-120 aft #01 J2334-160 bef #01 J2334-160 bef-2 120 160 160 #01 J2334-160 aft #02 J2334-160i 160 0 #02 J2334-120 bef #02 J2334-120 bef-2 120 120 #02 J2334-120 aft #02 J2334-160 bef #02 J2334-160 bef-2 120 160 160 #02 J2334-160 aft #03 160A&B @ Initial 160 0 #03 120A&B @120+J400 #03 120A&B @ 120 cycles final 120 120 #03 120A&B @ 120 cycles final 2 120 #03 160A&B @160 cycles final 160 After gravel, before cleaning After cleaning (flange view) After cleaning (flange view) After cleaning (flange view) #03 160A&B @160 cycles final 2 160 After cleaning (flange view) After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel PHOTO LIBRARY – LISTING 2 50 Cyclic Corrosion Test Specimens. (for photos see file: Photo Library-Cyclic Test) 2-A ID# in Report 4 5 Test Material HD Aluminized - Cr6 Austenitic Stainless and Neukote Pre-painted steels (continued) Photo ID Code #04 J2334-160i Exposure, cycles 0 #04 J2334-120 bef #04 J2334-120 bef-2 120 120 #04 J2334-120 aft #04 J2334-160 bef #04 J2334-160 bef-2 120 160 160 #04 J2334-160 aft 160 #11 J2334-160i 0 #11 J2334-120 bef #11 J2334-120 bef-2 120 120 #11 J2334-120 aft #11 J2334-160 bef #11 J2334-160 bef-2 120 160 160 #11 J2334-160 aft 160 Condition After gravel After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning PHOTO LIBRARY – LISTING 2 (continued) 51 PHOTO LIBRARY – LISTING 2 (continued) Cyclic Corrosion Test Specimens. (for photos see file: Photo Library-Cyclic Test) 2-B ID# in Report 6 7 8 Test Material HD Terne HD Tin-Zinc HD Aluminized Post-painted steels Photo ID Code #05 J2334-160i Exposure, cycles 0 #05 J2334-120 bef #05 J2334-120 bef-2 120 120 #05 J2334-120 aft #05 J2334-160 bef #05 J2334-160 bef-2 120 160 160 #05 J2334-160 aft #06 J2334-160i 160 0 #06 J2334-120 bef #06 J2334-120 bef-2 120 120 #06 J2334-120 aft #06 J2334-160 bef #06 J2334-160 bef-2 120 160 160 #06 J2334-160 aft #09 J2334-160i 160 0 #09 J2334-120 bef #09 J2334-120 bef-2 120 120 #09 J2334-120 aft #09 J2334-160 bef #09 J2334-160 bef-2 120 160 160 #09 J2334-160 aft 160 Condition After gravel After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning PHOTO LIBRARY – LISTING 2 (continued) 52 PHOTO LIBRARY – LISTING 2 (continued) Cyclic Corrosion Test Specimens. (for photos see file: Photo Library-Cyclic Test) 2-B ID# in Report 9 Test Material Ferritic Stainless Post-painted steels (continued) Photo ID Code #13 J2334-160i Exposure, cycles 0 #13 J2334-120 bef #13 J2334-120 bef-2 120 120 #13 J2334-120 aft #13 J2334-160 bef #13 J2334-160 bef-2 120 160 160 #13 J2334-160 aft 160 2-C ID# in Report 10 Test Material Austenitic Stainless Condition After gravel After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning Bare steels Photo ID Code #10 J2334-160i Exposure, cycles 0 #10 J2334-120 bef #10 J2334-120 bef-2 120 120 #10 J2334-120 aft #10 J2334-160 bef #10 J2334-160 bef-2 120 160 160 #10 J2334-160 aft 160 Condition After gravel After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning After gravel, before cleaning After gravel, before cleaning (flange view) After cleaning PHOTO LIBRARY – LISTING 2 (continued) 53 PHOTO LIBRARY – LISTING 3 Fuel Test Specimens. (for photos see file: Photo Library-Fuel Test) 3A ID# in Report 1 2 3 4 5 Pre-painted steels Test Material EG Zinc-Nickel + Cr6 EG Zinc-Nickel - Cr6 HDGA (Zinc-Iron) - Cr6 HD Aluminized + Cr6 Austenitic 304L Stainless with Neukote Photo ID Code #01 Initial Fuel Exposure Time, weeks 0 #01 @ 28 weeks 28 #01 @ 39 weeks 39 #02 Initial 0 #02 @ 28 weeks 28 #02 @ 39 weeks 39 #03 Initial 0 #03 @ 28 weeks 28 #03 @39 weeks 39 #04 Initial 0 #04 @ 28 weeks 28 #04 @ 39 weeks 39 #11 Initial 0 #11 @ 28 weeks 28 #11 @ 39 weeks 39 PHOTO LIBRARY – LISTING 3 54 PHOTO LIBRARY – LISTING 3 (continued) Fuel Test Specimens. (for photos see file: Photo Library-Fuel Test) 3-B ID# in Report 6 7 8 9 Post-painted steels Test Material HD Terne HD Tin-Zinc HD Aluminized Ferritic 436L Stainless 3C ID# in Report 10 Test Material Austenitic 304L Stainless Photo ID Code #05 Initial Fuel Exposure Time, weeks 0 #05 @ 28 weeks 28 #05 @ 39 weeks 39 #06 Initial 0 #06 @ 28 weeks 28 #06 @ 39 weeks 39 #09 Initial 0 #09 @ 28 weeks 28 #09 @ 39 weeks 39 #13 Initial 0 #13 @ 28 weeks 28 #13 @ 39 weeks 39 Bare steels Photo ID Code #10 Initial Fuel Exposure Time, weeks 0 #10 @ 28 weeks 28 #10 @ 39 weeks 39 PHOTO LIBRARY – LISTING 3 (continued) 55 APPENDIX 1 APPENDIX 1. Published data concerning the practical use and predictability of the Cyclic Corrosion test for automobile corrosion resistance were selected data from: “Perforation Corrosion Performance of Auto Body Steel Sheet in On-Vehicle and Accelerated Tests,” Dennis Davidson, Larry Thompson, Frank Lutze, Butch Tiburcio, Kevin Smith, Cindy Meade, Tom Mackie, Duncan McCune, Herb Townsend, Rebecca Tuszynski, and Martin Stephens, SAE 2003-01-1238 56 APPENDIX 1 (cont.) 57 APPENDIX 2 ID Pre-painted Steels 1- EG Zinc-Nickel with Cr6 Dome White Red 2- EG Zinc-Nickel without Cr6 3 HDGA without Cr6 4- HDAl with Cr6 5- Austenitic 304L + Neukote Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Aℓ 9- Ferritic 436L Bare steel 10- Austenitic 304L Scribe White Red Chip White Red Field White Red Region of Specimen Flange Flange (Under Clip) Weld White Red White Red White Red S S S M M M P P S M M M N N N N N N S N S S S S P S S N N N S S S S S S P P P S S S N N N N N N N N N N N N N N N N N N S S S S S S P P P S S S N N N N N N N N N S S S N N N N N N S S S S S S P P P S S S N N N N N N N N N S S S S N N N N N N N N N N N S S S N N N N N N N N N N N N N N N N N N N N N N N N N N N S N N N S N N N N N N N N N N N N N N S N N N N N N N N N N N N N N S S N N N N N N N N N N N N N S S N N S N N N N N N N N N N S S N S N N N N N N N N N N N S N N N N N N N N N N S M S M M M N N N N N N P P P N N N N N N N N N N N N S S S S S S N N N P P S N N N N N N N N N S S S S S S N N N N N N P P P N N N N N N N N N S S S S S S N N N N N N P P P N N N N N N N N N S S S S S S N N N N N N M M M N N N N N N N N N S S S S S S N N N N N N M M M N N N N N N N N N S S S S S S N N N N N N S S S N N N N N N N N N S S S S S S N N S N N N S S N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N S S S N N N S S S N N N S S S Key N S M P = = = = Weld (Under Clip) White Red None: no corrosion Slight: Less than approximately 15% corrosion Moderate: Approximately 15 – 30% corrosion Pronounced: Greater than approximately 30% corrosion APPENDIX 2. Visual ratings of rust after 2000 hours exposure in the Neutral Salt Spray Test. (Rust staining is not included in the ratings) Loss of Adhesion Note 1 Note 1 Note 2 Note 2 Notes A,C,D Notes A,B,D Notes A,B,D Note 3 Note 3 Note 3 Note 4 Note 4 Note 4 Note 5 Notes 5 & 6 Note 5 Notes 1. Moderate loss of adhesion in flange area A: Slight adhesion loss at dome 2. Pronounced adhesion loss in flange area B: Slight adhesion loss at flange/clip 3. Pronounced adhesion loss in flange area C: Moderate adhesion loss at flange/clip 4. Pronounced loss of adhesion/blistering in all areas D: Pronounced blistering at flange/clip 5. Pronounced loss of adhesion on flange underside and moderate loss of adhesion at scribe 58 6. Moderate loss of adhesion at chip area APPENDIX 3 Initial Weight ID Pre-painted steels 1- Eg Zinc-Nickel 338.4 g 1- + Cr6 338.4 1339.3 Final Weight Weight loss (gain), g Specific Average Average Weight Loss (Gain) % 337.7 g 337.8 338.9 0.7 0.6 0.4 0.6 0.2 0.9 0.3 (0.5) (0.2) 2- Eg Zinc-Nickel 2- - Cr6 2- 347.7 348.3 349.2 347.6 347.0 348.0 0.1 1.3 1.2 3- HDGA 3- - Cr6 3- 258.8 266.3 264.0 259.3 267.0 264.2 (0.5) (0.7) (0.2) 4- HDAl 4- + Cr6 4- 295.2 290.0 291.8 291.0 287.9 288.3 4.2 2.1 3.5 3.3 1.1 5- Austenitic 5- 304L 5- + Neukote 294.4 297.3 298.2 292.8 295.6 296.3 1.6 1.7 1.9 1.7 0.6 Post-painted steels 6- HD Terne 66- 314.9 313.6 319.6 314.9 313.6 319.5 0.0 0.0 0.1 0.0 0.0 7- HD Tin-Zinc 77- 320.3 326.3 322.8 320.5 326.2 322.9 0.2 0.1 0.1 0.1 0.0 8- HD Aluminum 88- 288.6 287.8 290.6 281.8 283.2 284.6 6.8 4.6 6.0 5.8+ 2.0 9- Ferritic 9- 436L 9- 265.6 265.2 271.2 264.1 262.6 269.7 1.5 2.6 1.5 1.9+ 0.7 Bare Steel 10- Austenitic 10- 304L 10- 290.5 293.0 292.7 289.8 292.3 291.9 0.7 0.7 0.8 0.7 0.2 + Weight losses were likely the result of paint loss. APPENDIX 3. Weight change of steel materials after 2000 hours exposure in the Neutral Salt Spray Test. 59 APPENDIX 4 Exposures 500 Steel 1 Steel 2 Zinc 1 Zinc 2 g 0.9000 0.8197 2.1446 3.2567 % 2.94 2.68 30.97 46.65 1000 g % 1.9058 6.22 1.9323 6.33 2.2287 32.08 3.3146 47.83 1500 g % 2.8908 9.43 2.9708 9.68 3.3118 47.88 3.6249 52.10 2000 g % 3.8758 12.6 4.0157 13.1 * * * * * Coupon disintegrated and could not be weighed. APPENDIX 4. Weight loss of test validation coupons in the Neutral Salt Spray Test. 60 APPENDIX 5 ID Pre-painted steels 1- EG Zn-Ni + Cr6 - Creepback from Scribe, mm Average Minimum Maximum Maximum Pit Depth (deeper than 0.1mm) 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None Observed None Observed None Observed 2- Eg Zn-Ni - Cr6 - 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None Observed None Observed None Observed 3- HDGA - Cr6 - 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None Observed None Observed None Observed 4- HDAl + Cr6 - 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None Observed None Observed None Observed 5- Austenitic - 304L + - Neukote 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None Observed None Observed None Observed Post-painted steels 6- HD Terne - 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None Observed None Observed None Observed 7- HD Tin-Zinc - 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None Observed None Observed None Observed 8- HD Aluminum - Full* Full* 12.2 Full* Full* 0.2 Full* Full* 62.2 None Observed None Observed None Observed 9- Ferritic - 436L Bare steel 10- Austenitic - 304L - 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None Observed None Observed None Observed 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None Observed None Observed None Observed * Loss of adhesion extended to edge of specimen APPENDIX 5. Creepback from scribe line and maximum pit depth for steels after exposure of 2000 hours in the Neutral Salt Spray test. 61 APPENDIX 6 ID 500 Hours Loss of Rating Adhesion 1000 Hours Loss of Rating Adhesion 1500 Hours Loss of Rating Adhesion 2000 Hours Loss of Rating Adhesion Pre-painted steels 1- EG Zn-Ni 5A 5A 5A 2- EG Zn-Ni 6A 6A 6A 3A- HDGA 6A 6A 6A 4- HD Alum. 6A 6A 6A 5- Austenitic 10 - 304L + 10 - Neukote 10 MC/T* MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None None 5A 5A 5A 6A 6A 6A 5A 6A 6A 6A 6A 6A 10 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None None 5A 5A 5A 6A 6A 6A 5A 6A 6A 6A 6A 6A 10 10 10 Post-painted steels 6- HD Terne 10 10 10 7- HD Tin-Zinc 10 10 10 8- HD Alum. 4A 4A 4A 9- Ferritic 5A - 436L 5A 5A None None None None None None MC/T MC/T MC/T S/T** S/T S/T 10 10 10 10 10 10 4A 4A 4A 4A 4A 4A None None None None None None MC/T MC/T MC/T S/T S/T S/T 10 None 10 None 10 None 10 None 10 None 10 None 10 None 10 None 10 None 10 None 10 None 10 None No rating due to excessive blistering " " " " " " " " 5B S/T 5B S/T 5B S/T 5B S/T 5B S/T 5B S/T None None None 10 10 10 Bare steel 10- Austenitic - 304L - 10 10 10 None None None 10 10 10 MC/T MC/T MC/T MC*/T MC*/T MC*/T MC*/T MC*/T MC*/T MC*/T MC*/T MC*/T None None None 5A 5A 5A 6A 6A 6A 5A 6A 6A 6A 6A 6A 10 10 10 None None None 10 10 10 Chip frequency Rating numbers 0 Number of chips >250 Loss of adhesion APPENDIX 6. 1 2 3 4 5 6 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None None None None None Size rating & size range of chips 7 8 9 10 150- 100755025105-9 2-4 1 0 250 159 99 74 49 24 *MC/T denotes Metallic Coating to topcoat / **S/T denotes Substrate steel to topcoat A B C D <1 mm 1-3 mm 3-6 mm >6 mm Gravelometer chip ratings of steel system specimens after 500 hours, 1000 hours, 1500 hours, and 2000 hours exposure in the Neutral Salt Spray Test. 62 APPENDIX 7 ID Pre-painted Steels 1- EG Zinc-Nickel 2- EG Zinc-Nickel 3- HDGA (Zn-Fe) 4- HDAl 5- Austenitic - 304L + Neukote Region of Specimen Dome Scribe Chip Field Flange Flange (Under Clip) Weld White Red White Red White Red White Red White Red White Red White Red Weld (Under Clip) White Red Loss of Adhesion S S S S M M S S N N S S N N S S S S N N S S S S S S S S N N N N S S P P S S N S S S S S M M S S N N S S S S S S N N S S S S S S M M N N N N N N N N S S N N N N N N N N N N N N N N N N N N S S N N S S N N N N N N N N N N N N N N N N N N S N N N N N M S N N N N S S N N M S N N S S N N N N S S N N N N M P N N S S N N S N Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Aluminized 9- Ferritic - 436L N N N N N N N N N N N N N N N N N N N N N N N N M M M M N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N M M N N N N N N P M N N N N N N N N N N N N N N N N N N N N N N S S N N N N N N S S N N N N N N N S N N N N N N N S N N Bare steel 10-Austenitic -304L N N N N N N S S N N S S N N N N N N S S N N S S N N M M N N S S N S M P = = = = None: no corrosion Slight: Less than approximately 15% corrosion Moderate: Approximately 15 – 30% corrosion Pronounced: Greater than approximately 30% corrosion Note 1 Note 1 Note 2 Note 2 Note 3 Note 3 Note 1: Moderate blistering in flange area Note 2: Moderate adhesion loss in chip area and slight loss of adhesion in scribe area Note 3: Moderate to Pronounced adhesion loss in all areas APPENDIX 7. Visual ratings of corrosion severity after 80 cycles exposure in the Cyclic Corrosion Test. 63 APPENDIX 8 ID Pre-painted Steels 1- EG Zinc-Nickel - Cr6 2- Eg Zinc-Nickel - Cr6 3- HDGA (Zn-Fe) 4- HDAl - Cr6 5- Austenitic - 304L + Neukote Region of Specimen Dome Scribe Chip Field Flange Flange (Under Clip) Weld Weld (Under Clip) White Red White Red White Red Loss of Adhesion White Red White Red White Red White Red White Red S S S S M M S S N N S S S S S S S S N N S S S S S S S S N N S S S S P P S S S S S S S S M M S S N N S S S S S S N N S S S S S S M M N N N N N N N N S S N N N N N N N N S S N N N N N N N N S S N N S S N N N N S S N N N N N N N N S S N N S S N N N S M S N N N N M M S N M S N N S S N N N N S S N N N N P P N N M S N N S S Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Aluminized 9- Ferritic - 436L N N N N N N N N S N N N N N N N N N N N N N N N M M M M N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N M M N N N N N N P P N N N N N N S S N N N N N N N N N N N N N N S S N N N N N N P P N N N N N N S S N N N N N N S S N N Bare steel 10-Austenitic -304L N N N N N N S S N N S S N N N N N N S S N N S S N N S M N N S S N S M P = = = = None: no corrosion Slight: Less than approximately 15% corrosion Moderate: Approximately 15 – 30% corrosion Pronounced: Greater than approximately 30% corrosion Note 1 Note 1 Note 2 Note 2 Note 3 Note 3 Note 1: Moderate blistering in flange area Note 2: Moderate adhesion loss in chip area and slight loss of adhesion in scribe area Note 3: Moderate to Pronounced adhesion loss in all areas APPENDIX 8. Visual ratings of corrosion severity after 120 cycles exposure in the Cyclic Corrosion Test. 64 APPENDIX 9 ID Pre-painted Steels 1- EG Zinc-Nickel - Cr6 2- Eg Zinc-Nickel - Cr6 3- HDGA (Zn-Fe) 4- HDAl - Cr6 5- Austenitic - 304L + Neukote Region of Specimen Dome Scribe Chip Field Flange Flange (Under Clip) Weld Weld (Under Clip) White Red White Red White Red Loss of Adhesion White Red White Red White Red White Red White Red S S S S M M S S N N S S N S S S M M N N S S S S S S S S N N S S S S P P S S S S S S S S M M S S N N S S S S S S N N S S S S S S M M N N N N N N N N S S N N N S N N N N S S N N N N N N N N M S N S S S N N N N N S N N N N N N N N S S N N S N N N N N S S N N N N P M S S P S S N M S N N N N S S N N N N N N N M P S N N S S Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Aluminized 9- Ferritic - 436L N N N N N N N N N N N N N N N N N N N N N N N N M M M M N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N N M M N N N N N N P P N N N N N N S S N N N N N N N S N N N N N N S S N N N N N N P P N N N N N N N S N N N N N N N S N N Bare steel 10-Austenitic -304L N N S N N N S S N N S S N N N N N N S S N N S S N N M M N N S S N S M P = = = = None: no corrosion Slight: Less than approximately 15% corrosion Moderate: Approximately 15 – 30% corrosion Pronounced: Greater than approximately 30% corrosion Note 1 Note 1 Note 2 Note 2 Note 3 Note 3 Note 1: Moderate blistering in flange area Note 2: Moderate adhesion loss in chip area and slight loss of adhesion in scribe area Note 3: Moderate to Pronounced adhesion loss in all areas APPENDIX 9. Visual ratings of corrosion severity after 160 cycles exposure in the Cyclic Corrosion Test. 65 APPENDIX 10 ID Pre-painted steels 1- EG Zinc-Nickel 2- EG Zinc-Nickel 3- HDGA (Zn-Fe) 4- HDAl 5- Austenitic - 304L + Neukote Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Aluminum 9- Ferritic - 436L Bare Steel 10- Austenitic - 304L Control (CRS) (6 specimens) Initial Weight Final Weight Change, g 336.3 338.4 345.7 348.5 258.1 261.3 286.9 286.6 297.1 295.9 336.1 338.3 345.6 348.3 258.7 261.6 286.9 286.7 295.9 294.7 -0.2 -0.1 -0.1 -0.2 0.6 0.3 0.0 0.1 -1.2 -1.2 311.7 321.7 323.7 330.0 290.4 290.1 263.1 264.4 312.1 322.2 324.0 330.5 290.3 290.0 270.6 269.6 0.4 0.5 0.3 0.5 -0.1 -0.1 7.5 5.2 289.9 289.7 175.2 297.0 297.0 42.1 7.1 7.3 1 33.1 Average % Change -0.15 -0.04 -0.15 -0.04 0.5 0.2 0.05 0.02 -1.2 -0.4 0.45 0.14 0.4 0.12 -0.1 -0.03 6.35 + 2.41+ 7.2+ 2.48+ 76.0 + The reason for the weight increases is unclear. APPENDIX 10. Weight change data for steel specimens and bare cold rolled steel (CRS) control after 80-cycle exposure in the Cyclic Corrosion test. 66 APPENDIX 11 ID Pre-painted steels 1- EG Zinc-Nickel 6 - Cr 2- EG Zinc-Nickel 6 - - Cr 3- HDGA (Zn-Fe) 4- HDAl - + Cr6 5- Austenitic - 304L + Neukote Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Aluminized 9- Ferritic - 436L Bare Steel 10-Austenitic -304L Control (CRS) + Initial Weight Final Weight Change, g 338.6 339.5 348.7 345.7 258.0 262.9 286.4 286.9 298.1 298.6 338.9 339.9 348.7 345.9 258.9 263.4 286.9 287.7 297.2 297.7 0.3 0.4 0.0 0.2 0.9* 0.5* 0.5 0.8 -0.9 -0.9 325.4 316.2 337.2 328.5 287.6 287.1 260.1 264.5 326.4 317.1 338.3 329.3 288.1 287.4 264.8 268.4 1.0 0.9 1.1 0.8 0.5 0.3 4.7 3.9 294.1 291.6 301.5 298.8 7.4 7.2 Average % Change 0.35 0.10 0.10 0.03 0.7 0.27 0.65 0.23 -0.90 -0.30 0.95 0.30 0.95 0.29 0.40 0.14 4.30 + 1.64+ 7.3+ 2.49+ Coupons removed after 80 cycles The reason for the weight increases is unclear. *Unable to remove all corrosion products with air blow-off APPENDIX 11. Weight change data for steel specimens after 120-cycle exposure in the Cyclic Corrosion test. 67 APPENDIX 12 ID Pre-painted steels 1- EG Zinc-Nickel 2- EG Zinc-Nickel 3- HDGA (Zn-Fe) 4- HDAl 5- Austenitic - 304L + Neukote Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Aluminum 9- Ferritic - 436L Bare Steel 10-Austenitic -304L Control (CRS) Initial Weight Final Weight Change, g 340.3 339.8 346.6 346.9 264.2 260.6 287.0 287.0 297.4 297.8 340.0 340.0 347.2 346.0 265.7 260.9 287.4 287.3 296.1 296.5 -0.3 0.2 0.6 -0.9 1.5 0.3 0.4 0.3 -1.3 -1.3 325.4 326.7 334.9 318.0 290.0 289.2 261.7 266.7 325.9 327.2 335.3 318.4 291.0 291.5 256.6 259.0 0.5 0.5 0.4 0.4 1.0 2.3 -5.1 -7.7 289.5 288.2 290.4 289.2 0.9 1.0 + Average % Loss (Gain) 0 0 -0.3 0.09 0.9 (0.3) 0.35 (0.12) -1.3 0.55 0.5 (0.15) 0.4 (0.12) 1.65 (0.57) -6.4 2.42 0.95 (0.33) + Coupons removed after 80 cycles Weight loss is attributed to loss of the paint film. APPENDIX 12. Weight change data for steel specimens after 160-cycle exposure in the Cyclic Corrosion test. 68 APPENDIX 13 Control Specimen* Initial Weight, g Final Weight, g Loss In Weight, g 1 176.4 32.7 143.7 2 173.1 37.3 135.8 3 175.4 46.8 128.6 4 174.7 47.4 127.3 5 175.9 50.5 125.4 6 175.7 37.9 137.8 Average 175.2 42.1 133.1 (76%) APPENDIX 13. Weight loss of bare cold rolled steel control samples after 80 cycles exposure in the Cyclic Corrosion test. 69 APPENDIX 14 Creepback from Scribe, mm Average Maximum Pit Depth,mm (above 0.1mm) Minimum Maximum 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None observed None observed 0.1 None observed None observed None observed 4- HDAl 0.0 0.0 0.0 5- Austenitic - 304L + Neukote 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.4 None observed None observed None Observed None Observed Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Aluminum 9- Ferritic - 436L 0.0 0.0 0.0 0.0 0.6 0.6 7.2 6.5 0.0 0.0 0.0 0.0 0.4 0.1 0.1 0.1 0.0 0.0 0.0 0.0 1.7 1.0 29.3 36.4 None Observed None Observed None Observed None Observed None Observed None Observed None Observed None Observed Bare steel 10-Austenitic -304L 0.0 0.0 0.0 0.0 0.0 0.0 None Observed None Observed ID Pre-painted steels 1- EG Zinc-Nickel 2- Eg Zinc-Nickel 3- HDGA (Zn-Fe) - Location of Pit Gravel area Other areas Gravel area APPENDIX 14. Creepback and maximum pit depths for steel test materials exposed for 80 cycles in the Cyclic Corrosion test. 70 APPENDIX 15 Creepback from Scribe, mm Minimum Maximum 0.0 0.0 0.0 0.0 0.0 0.0 2- Eg Zinc-Nickel 3- HDGA (Zn-Fe) - 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 4- HDAl 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.4 0.4 No rating* No rating* 0.0 0.0 0.0 0.0 0.1 0.1 No rating* No rating* 0.0 0.0 0.0 0.0 ID Pre-painted steels 1- EG Zinc-Nickel - 5- Austenitic - 304L + Neukote Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Aluminum 9- Ferritic - 436L Bare steel 10-Austenitic -304L Average 0.0 0.0 0.0 0.0 0.9 0.8 No rating* No rating* 0.0 0.0 Pit Depth and Location Maximum Pit Depth,mm (above 0.1mm) Location of Pit 0.2 None observed 0.2 None observed None observed None observed None observed None observed Gravel area Other areas Gravel area Other areas 0.4 None observed 0.2 None observed None Observed None Observed Gravel area Other areas Gravel area Other areas None Observed None Observed None Observed None Observed None Observed None Observed None Observed None Observed None Observed None Observed * Unable to rate due to pronounced adhesion loss. APPENDIX 15. Creepback and maximum pit depths for steel test materials exposed for 120 cycles in the Cyclic Corrosion test. 71 APPENDIX 16 Creepback from Scribe, mm Maximum Pit Depth,mm (deeper than 0.1mm) ID Pre-painted steels 1- EG Zinc-Nickel 6 - + Cr Average Minimum 0.0 0.0 0.0 0.0 0.0 0.0 None observed None observed 2- Eg Zinc-Nickel - - Cr6 3- HDGA (Zn-Fe) 4- HDAl - + Cr6 5- Austenitic - 304L + Neukote 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 None observed None observed None observed None observed None observed None observed None Observed None Observed 0.0 0.0 0.0 0.0 0.1 0.2 0.1 No rating* 0.0 0.0 0.0 0.0 1.0 1.4 17.6 No rating* None Observed None Observed None Observed None Observed None Observed None Observed None Observed None Observed 0.0 0.0 0.0 0.0 None Observed None Observed Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Aluminum 9- Ferritic - 436L Bare steel 10-Austenitic -304L 0.0 0.0 0.0 0.0 0.4 0.6 2.5 No rating* 0.0 0.0 Maximum * Unable to rate due to pronounced adhesion loss. APPENDIX 16. Creepback and maximum pit depths for steel test materials exposed for 160 cycles in the Cyclic Corrosion test. 72 APPENDIX 17 20 Cycles Loss of Rating Adhesion ID Pre-painted steels 1- EG Zinc-Nickel 5A MC/T* 6 5A MC/T - + Cr 2- EG Zinc-Nickel 5A MC/T 6 5A MC/T - - Cr 3- HDGA (Zn-Fe) 6A MC/T 6A MC/T 4- HD Alum. 6A MC/T 6 6A MC/T - + Cr 5- Austenitic 10 None - 304L+Neukote 10 None 40 Cycles Loss of Rating Adhesion 60 Cycles Loss of Rating Adhesion 80 Cycles Loss of Rating Adhesion 5A 5A 5A 5A 5A 5A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 4A 4A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 4A 4A 6A 6A 8A 6A MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T S/T** S/T Post-painted steels 6- HD Terne 10 10 7- HD Tin-Zinc 10 10 8- HD Alum. 5A 5A 9- Ferritic 6B - 436L 6B None None None None MC/T MC/T S/T S/T 10 10 10 10 6B 6B 6B 6B None None None None MC/T MC/T S/T S/T 10 10 10 10 6B 6B 4C 4C None None None None MC/T MC/T S/T S/T 10 10 10 10 5C 5C 4C 4C None None None None MC/T MC/T S/T S/T Bare steel 10-Austenitic -304L None None 10 10 None None 10 10 None None 10 10 None None 10 10 Chip frequency Rating numbers 0 Number of chips >250 Loss of adhesion 1 2 3 4 5 6 Size rating & size range of chips 7 8 9 150- 100755025105-9 2-4 1 250 159 99 74 49 24 *MC/T denotes Metallic Coating to topcoat / **S/T denotes steel to topcoat 10 A B C D 0 <1 mm 1-3 mm 3-6 mm >6 mm APPENDIX 17. Gravelometer chip ratings for the 80 cycles exposure set of all steel specimens 73 APPENDIX 18 20 Cycles Loss of Rating Adhesion ID Pre-painted steels 1- EG Zinc-Nickel 6 - + Cr 2- EG Zinc-Nickel 6 - - Cr 3- HDGA (Zn-Fe) 4- HD Alum. 6 - + Cr 5- Austenitic - 304L+Neukote Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Alum. 9- Ferritic - 436L Bare steel 10-Austenitic -304L 60 Cycles Loss of Rating Adhesion 5A 5A 5A 5A 6A 6A 6A 6A 10 10 MC/T* MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 5A 5A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 4A 4A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 10 10 10 10 5A 5A 6B 6B None None None None MC/T MC/T S/T** S/T 10 10 10 10 6B 6B 6B 6B None None None None MC/T MC/T S/T S/T 10 10 10 10 6B 6B 4C 4C None None None None MC/T MC/T S/T S/T 10 10 None None 10 10 None None 10 10 None None 80 Cycles Loss of Rating Adhesion ID Pre-painted steels 1- EG Zinc-Nickel 6 - + Cr 2- EG Zinc-Nickel 6 - - Cr 3- HDGA (Zn-Fe) 4- HD Alum. 6 - + Cr 5- Austenitic - 304L+Neukote Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Alum. 9- Ferritic - 436L Bare steel 10-Austenitic -304L 40 Cycles Loss of Rating Adhesion 100 Cycles Loss of Rating Adhesion 120 Cycles Loss of Rating Adhesion 5A 5A 5A 5A 4A 4A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 4A 4A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 4A 4A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T S/T S/T 10 10 10 10 6B 6B 4C 4C None None None None MC/T MC/T S/T S/T 10 10 10 10 6B 6B 4C 4C None None None None MC/T MC/T S/T S/T 10 10 10 10 4C 5C 2C 2C None None None None MC/T MC/T S/T S/T 10 10 None None 10 10 None None 10 10 None None Chip frequency Rating numbers Number of chips Loss of adhesion 0 >250 1 2 3 4 5 6 7 8 9 150- 100755025105-9 2-4 1 250 159 99 74 49 24 *MC/Tdenotes Metallic Coating to topcoat / **S/T denotes steel to topcoat Size rating & size range of chips 10 0 A <1 mm B 1-3 mm C 3-6 mm D >6 mm APPENDIX 18. Gravelometer chip ratings for the 120 cycles exposure set of all steel specimens 74 APPENDIX 19 20 Cycles Loss of Rating Adhesion ID Pre-painted steels 1- EG Zinc-Nickel 6 - + Cr 2- EG Zinc-Nickel 6 - - Cr 3- HDGA (Zn-Fe) 4- HD Alum. 6 - + Cr 5- Austenitic - 304L+Neukote Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Alum. 9- Ferritic - 436L Bare steel 10- Austenitic - 304L 40 Cycles Loss of Rating Failure 80 Cycles Loss of Rating Adhesion 5A 5A 5A 5A 6A 6A 6A 6A 10 10 MC/T* MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 5A 5A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 4A 4A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 4A 4A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 10 10 10 10 5A 5A 6B 6B None None None None MC/T MC/T ** S/T S/T 10 10 10 10 6B 6B 6B 6B None None None None MC/T MC/T S/T S/T 10 10 10 10 6B 6B 4C 4C None None None None MC/T MC/T S/T S/T 10 10 10 10 6B 6B 4C 4C None None None None MC/T MC/T S/T S/T 10 10 None None 10 10 None None 10 10 None None 10 10 None None 100 Cycles Loss of Rating Adhesion ID Pre-painted steels 1- EG Zinc-Nickel 6 - + Cr 2- EG Zinc-Nickel 6 - - Cr 3- HDGA (Zn-Fe) 4- HD Alum. 6 - + Cr 5- Austenitic - 304L+Neukote Post-painted steels 6- HD Terne 7- HD Tin-Zinc 8- HD Alum. 9- Ferritic - 436L Bare steel 10-Austenitic -304L 60 Cycles Loss of Rating Adhesion 120 Cycles Loss of Rating Adhesion 140 Cycles Loss of Rating Adhesion 5A 5A 5A 5A 4A 4A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 4A 4A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 4A 4A 6A 6A 10 10 MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T None None 5A 5A 5A 5A 4A 4A 6A 6A 6B 4A MC/T MC/T MC/T MC/T MC/T MC/T MC/T MC/T S/T S/T 10 10 10 10 6B 6B 2C 2C None None None None MC/T MC/T S/T S/T 10 10 10 10 6B 6B 2C 2C None None None None MC/T MC/T S/T S/T 10 10 10 10 4B 4B 2C 2C None None None None MC/T MC/T S/T S/T 10 10 10 10 4C 4C 2C 2C None None None None MC/T MC/T S/T S/T 10 10 None None 10 10 None None 10 10 None None 10 10 None None Chip frequency Rating numbers 0 Number of chips >250 Loss of adhesion 160 Cycles Loss of Rating Adhesion 1 2 3 4 5 6 Size rating & size range of chips 7 8 9 150- 100755025105-9 2-4 1 250 159 99 74 49 24 *MC/T denotes Metallic Coating to topcoat / **S/T denotes steel to topcoat 10 A B C D 0 <1 mm 1-3 mm 3-6 mm >6 mm APPENDIX 19. Gravelometer chip ratings for the 160 cycles exposure set of all steel specimens 75 APPENDIX 20 Extent of white residue Steel ID Lid (Vapor Area) Vapor area Cup Interface Area Fuel Area Pre-painted steel category +6 N N N N 1 – EG Zinc-Nickel (with Cr ) – N N N N – N S N N 2 – EG Zinc-Nickel (without Cr+6) N N N N – N N N N – N N N N 3 – HDGA Zn-Fe (without Cr+6) N N N N – N N N N – N N N N 4 – HDAℓ (with Cr+6) N N N N – N N N N – N N N N 5 – Austenitic 304L Stainless (Neukote) N N N N – N N N N – N N N N Post-painted steel category 6 – HD Terne N N N N – N N N N – N N N N 7 – HD Tin-Zinc N N N N – N N N N – N N N N 8 – HD Aluminized N N N N – N N N N – N N N N 9 – Ferritic 436L Stainless N N N N – N N N N – N N N N Bare steel category 10 – Austenitic 304L Stainless N N N N – N N N N – N N N N N = None; S = Slight (<15% of area); M = Moderate (15-30% of area); P = Pronounced (>30% of area) APPENDIX 20. Extent of white residue and observations after 4 weeks. 76 APPENDIX 21 Extent of white residue Steel ID Lid (Vapor Area) Cup Interface Area Fuel Area Pre-painted steel category 1 – EG Zinc-Nickel (with Cr+6) N N N N – N N N N – N S N N 2 – EG Zinc-Nickel (without Cr+6) N N N N – N N N N – N N N N 3 – HDGA Zn-Fe (without Cr+6) N S N N – N S N N – N S N N 4 – HDAℓ (with Cr+6) N N N N – N N N N – N N N N 5 – Austenitic 304L Stainless (Neukote) N N N N – N N N N – N N N N Post-painted steel category 6 – HD Terne N N N N – N N N N – N N N N 7 – HD Tin-Zinc N N N N – N N N N – N N N N 8 – HD Aluminized N N N N – N N N N – N N N N 9 – Ferritic 436LStainless N N N N – N N N N – N N N N Bare steel category 10 – Austenitic 304L Stainless N N N N – N N N N – N N N N N = None; S = Slight (<15% of area); M = Moderate (15-30% of area); P = Pronounced (>30% of area) APPENDIX 21. Vapor area Extent of white residue and observations after 8 weeks. 77 APPENDIX 22 Extent of white residue Steel ID Lid (Vapor Area) Vapor area Cup Interface Area Fuel Area Pre-painted steel category +6 N N N N 1 – EG Zinc-Nickel (with Cr ) – N S N N – N S N N 2 – EG Zinc-Nickel (without Cr+6) N N N N – N N N N – N N N N 3 – HDGA Zn-Fe (without Cr+6) N N N N – N N N N – N N N N 4 – HDAℓ (with Cr+6) N N N N – N N N N – N N N N 5 – Austenitic 304L Stainless (Neukote) N N N N – N N N N – N N N N Post-painted steel category 6 – HD Terne N N N N – N N N N – N N N N 7 – HD Tin-Zinc N N N N – N N N N – N N N N 8 – HD Aluminized N N N N – N N N N – N N N N 9 – Ferritic 436L Stainless N N N N – N N N N – N N N N Bare steel category Slight darkening 10 – Austenitic 304L Stainless N N N Slight darkening – N N N Slight darkening – N N N N = None; S = Slight (<15% of area); M = Moderate (15-30% of area); P = Pronounced (>30% of area) APPENDIX 22. Extent of white residue and observations after 12 weeks. 78 APPENDIX 23 Extent of white residue Steel ID Pre-painted steel category +6 1 – EG Zinc-Nickel (with Cr ) – – 2 – EG Zinc-Nickel (without Cr+6) – – 3 – HDGA Zn-Fe (without Cr+6) – – 4 – HDAℓ (with Cr+6) – – 5 – Austenitic 304L Stainless Neukote) – – Post-painted steel category 6 – HD Terne – – 7 – HD Tin-Zinc – – 8 – HD Aluminized – – 9 – Ferritic 436L Stainless – – Bare steel category 10 – Austenitic 304L Stainless – – Lid (Vapor Area) Vapor area Cup Interface Area Fuel Area N N N N N N N N N N N N N N N N S S N N N N N N N N N N N N N N N N N N N N N N N N N M M N N N N N N N N N N N N N N N N S S N N N N N N N N N N S S N N N N N N N N N M M P M M M P M M P P P N N N N N N N N N N N N N N N N N N M M M Slight darkening Slight darkening Slight darkening N = None; S = Slight (<15% of area); M = Moderate (15-30% of area); P = Pronounced (>30% of area) APPENDIX 23. Extent of white residue and observations after 16 weeks. 79 APPENDIX 24 Extent of white residue Steel ID Pre-painted steel category +6 1 – EG Zinc-Nickel (with Cr ) – – 2 – EG Zinc-Nickel (without Cr+6) – – 3 – HDGA Zn-Fe (without Cr+6) – – 4 – HDAℓ (with Cr+6) – – 5 – Austenitic 304L Stainless (Neukote) – – Post-painted steel category 6 – HD Terne – – 7 – HD Tin-Zinc – – 8 – HD Aluminized – – 9 – Ferritic 436L Stainless – – Bare steel category 10 – Austenitic 304L Stainless – – Lid (Vapor Area) Vapor area Cup Interface Area Fuel Area N S S N N N N N N N N N N N N N N N N N N N N N N N N N M P N N N N N N N N N N N N N N N N S S N S S N N N N N N N M M N N N N N N N N N P P P P M M P M M P P P N N N S S S N N N N N N N N N N N N M P P Slight darkening Slight darkening Slight darkening N N (1 red point) N N N N N N N N N N N N N N = None; S = Slight (<15% of area); M = Moderate (15-30% of area); P = Pronounced (>30% of area) APPENDIX 24. Extent of white residue and observations after 20 weeks. 80 APPENDIX 25 Extent of white residue Steel ID Pre-painted steel category 1 – EG Zinc-Nickel (with Cr+6) – – 2 – EG Zinc-Nickel (without Cr+6) – – 3 – HDGA Zn-Fe (without Cr+6) – – 4 – HDAℓ (with Cr+6) – – 5 – Austenitic 304L Stainless (Neukote) – – Post-painted steel category 6 – HD Terne – – 7 – HD Tin-Zinc – – 8 – HD Aluminized – – 9 – Ferritic 436L Stainless – – Bare steel category 10 – Austenitic 304L Stainless – – Lid (Vapor Area) Vapor area Cup Interface Area Fuel Area N S S N S N S S S N N N S S S N N N N N N N N N N N N M M P N N N N N N N N N N N N N N P N S S P M M N N N N N N S M M N N N N N N N N N P P P M M M P P P P P P S S S S S S N N N N N N N N N N N N M P P Slight darkening Slight darkening Slight darkening N N (1 red point) N N N N N N N N N N N N S N = None; S = Slight (<15% of area); M = Moderate (15-30% of area); P = Pronounced (>30% of area) APPENDIX 25. Extent of white residue and observations after 24 weeks. 81 APPENDIX 26 Extent of white residue Steel ID Pre-painted steel category 1 – EG Zinc-Nickel (with Cr+6) – – Lid (Vapor Area) Vapor area Cup Interface Area Fuel Area N N N N N N N N N N N N S N S S N N N N N N S S N S S S N N N S S S N N N N N N N N N M P P N N N N N N N N N N N P S S S P M M N N N N N N S M M N N N N N N N N N P P P P P P P P P P P P S S S S S S N N N N N N N N (1 red point) 2 – EG Zinc-Nickel (without Cr+6) – – 3 – HDGA Zn-Fe (without Cr+6) – – 4 – HDAℓ (with Cr+6) – – 5 – Austenitic 304L Stainless (Neukote) – – Post-painted steel category 6 – HD Terne – – 7 – HD Tin-Zinc – – 8 – HD Aluminized – – 9 – Ferritic 436L Stainless – – Bare steel category 10 – Austenitic 304L Stainless – – N = None; S = Slight (<15% of area); Slight darkening N N P Slight darkening N N P Slight darkening N N P M = Moderate (15-30% of area); P = Pronounced (>30% of area) APPENDIX 26. Extent of white residue and observations after 28 weeks. 82 APPENDIX 27 Extent of white residue Steel ID Pre-painted steel category +6 1 – EG Zinc-Nickel (with Cr ) – – 2 – EG Zinc-Nickel (without Cr+6) – – 3 – HDGA Zn-Fe (without Cr+6) – – 4 – HDAℓ (with Cr+6) – – 5 – Austenitic 304L Stainless (Neukote) – – Post-painted steel category 6 – HD Terne – – 7 – HD Tin-Zinc – – 8 – HD Aluminized – – 9 – Ferritic 436L Stainless – – Bare steel category 10 – Austenitic 304L Stainless – – Lid (Vapor Area) Vapor area Cup Interface Area Fuel Area N N N N N N N N N N S S S S S S N N N N N N S S N S S S N N N S S S N N N N N N N N N M P P N N N N N N N N N N N P S S S P M M N N N N N N S P P S S S N N N N N N P P P P P P P P P P P P S S S S S S N N N N N N N N N N N N P P P Slight darkening Slight darkening Slight darkening N N (1 red point) N = None; S = Slight (<15% of area); M = Moderate (15-30% of area); P = Pronounced (>30% of area) APPENDIX 27. Extent of white residue and observations after 32 weeks. 83 APPENDIX 28 Extent of white residue Steel ID Pre-painted steel category +6 1 – EG Zinc-Nickel (with Cr ) – – Lid (Vapor Area) N N (1 red point) Vapor area Cup Interface Area Fuel Area N S S N N N N N N N 2 – EG Zinc-Nickel (without Cr+6) N S N N – N S N N – N N N N 3 – HDGA Zn-Fe (without Cr+6) N S N N – N S N N – N S N N 4 – HDAℓ (with Cr+6) N N N N – N N N N – N N N N 5 – Austenitic 304L Stainless (Neukote) S S M N – S S P N – S S P P Post-painted steel category 6 – HD Terne S S P S – S P P S – S P P S 7 – HD Tin-Zinc P S P S – M S P S – M S P S 8 – HD Aluminized N N P N – N N P N – N N P N 9 – Ferritic 436L Stainless N N P N – N N P N – N N P N Bare steel category Slight darkening 10 – Austenitic 304L Stainless N N P Slight darkening – N N P Slight darkening – N N P N = None; S = Slight (<15% of area); M = Moderate (15-30% of area); P = Pronounced (>30% of area) APPENDIX 28. Extent of white residue and observations after 36 weeks. 84 APPENDIX 29 Extent of white residue Steel ID Pre-painted steel category +6 1 – EG Zinc-Nickel (with Cr ) – – 2 – EG Zinc-Nickel (without Cr+6) – – 3 – HDGA Zn-Fe (without Cr+6) – – 4 – HDAℓ (with Cr+6) – – 5 – Austenitic 304L Stainless (Neukote) – – ost-painted steel category 6 – HD Terne – – 7 – HD Tin-Zinc – – 8 – HD Aluminized – – 9 – Ferritic 436L Stainless – – Bare steel category 10 – Austenitic 304L Stainless – – Lid (Vapor Area) Vapor area Cup Interface Area Fuel Area N N N N N N N N N N S S S S S S N N N N N N S S S S S S N N N S S S N N N N N N N N N P P P N N N N N N N N N N N P S S M P M M N N N N N N S P P S S S N N N N N N P P P P P P P P P P P P S P P S S S N N N N N N N N N N N N P P P Slight darkening Slight darkening Slight darkening N N (1 red point) N = None; S = Slight (<15% of area); M = Moderate (15-30% of area); P = Pronounced (>30% of area) APPENDIX 29. Extent of white residue and observations after 39 weeks. 85 ID Prepaint Postpaint Bare APPENDIX 30 Exposure time, weeks INITIAL 4 8 12 16 20 24 28 32 36 39 1-1 EG Zn-Ni 1-2 +Cr6 1-3 2-1 EG Zn-Ni 2-2 -Cr6 2-3 3-1 HDGA 3-2 -Cr6 3-3 4-1 HDAℓ 4-2 +Cr6 4-3 5-1 Stainless 5-2 5-3 58.7196 59.5354 59.1027 61.108 61.2032 60.2463 50.1409 50.8337 50.6874 56.1806 56.2672 56.1086 69.8092 69.7561 69.4543 58.7273 59.5435 59.1068 61.1135 61.2064 60.2552 50.1062 50.8008 50.6536 56.185 56.2745 56.1078 69.8256 69.7669 69.4563 58.7222 59.5401 59.1045 61.1103 61.2056 60.251 50.0978 50.794 50.6453 56.179 56.2671 56.1022 69.8222 69.7632 69.4569 58.72 59.5362 59.103 61.1095 61.2043 60.2481 50.0946 50.7936 50.6413 56.1755 56.2655 56.1008 69.8204 69.7628 69.4569 58.7178 59.5349 59.1008 61.1081 61.2025 60.2463 50.0905 50.7891 50.6401 56.174 56.2632 56.0999 69.82 69.7625 69.4555 58.7182 59.5354 59.1025 61.1095 61.2036 60.2479 50.091 50.7915 50.6397 56.1765 56.2639 56.1011 69.8187 69.7617 69.4555 58.7173 59.5346 59.1023 61.1076 61.2033 60.247 50.0919 50.7891 50.6376 56.1765 56.2638 56.1012 69.8193 69.7621 69.4566 58.7169 59.5339 59.1016 61.1073 61.2027 60.2461 50.0866 50.7876 50.6377 56.1762 56.2627 56.0993 69.8181 69.7611 69.4561 58.7182 59.5362 59.1033 61.1094 61.2031 60.246 50.0875 50.7877 50.639 56.1764 56.2652 56.1016 69.8186 69.7618 69.4567 58.7172 59.534 59.1012 61.1074 61.2025 60.2461 50.0858 50.7859 50.6344 56.1766 56.2636 56.1004 69.8194 69.7608 69.4563 58.7143 59.5312 59.0974 61.1033 61.1976 60.2422 50.0802 50.7798 50.6291 56.1725 56.2588 56.0961 69.8172 69.7608 69.4563 6-1 HD Terne 6-2 6-3 7-1 HDSn-Zn 7-2 7-3 8-1 HDAℓ 8-2 8-2 9-1 Fe Stain 9-2 9-3 10-1 304L Stain 10-2 10-3 51.1515 51.1739 51.1658 51.3344 51.3981 51.334 54.6739 54.7048 54.591 50.8958 50.8646 50.745 69.0016 69.0689 69.1909 51.1531 51.1704 51.1641 51.3329 51.4003 51.3361 54.6734 54.7061 54.5897 50.8946 50.8674 50.7452 69.0002 69.0727 69.1884 51.149 51.1696 51.1632 51.3327 51.398 51.3332 54.6727 54.7038 54.5831 50.8931 50.8654 50.7457 68.9998 69.0714 69.1892 51.147 51.1686 51.1626 51.333 51.398 51.3339 54.6731 54.703 54.5833 50.892 50.8656 50.7454 68.9983 69.0704 69.1881 51.1466 51.1672 51.1622 51.3314 51.3978 51.3317 54.6719 54.7038 54.5823 50.8955 50.8651 50.7459 68.9991 69.0707 69.1893 51.1454 51.1674 51.1608 51.3309 51.3973 51.3322 54.6716 54.7034 54.5823 50.893 50.8661 50.744 68.9996 69.0697 69.1889 51.1429 51.1682 51.1601 51.3307 51.3971 51.3316 54.6728 54.7039 54.5821 50.8959 50.8653 50.7451 68.9995 69.0705 69.1892 51.1363 51.1655 51.16 51.3308 51.3965 51.331 54.6721 54.7037 54.5828 50.8949 50.8662 50.7452 69.0002 69.0698 69.1892 51.1349 51.1625 51.1595 51.3302 51.3959 51.3309 54.6726 54.7038 54.5828 50.8944 50.8645 50.7447 69.0006 69.0704 69.189 51.1318 51.1601 51.157 51.329 51.3949 51.3313 54.6728 54.7038 54.5824 50.8953 50.8645 50.7458 69.0018 69.0709 69.1906 51.1299 51.1572 51.1552 51.3294 51.3946 51.3303 54.6732 54.7047 54.5829 50.8956 50.8663 50.7481 69.0003 69.0702 69.1894 APPENDIX 30. Actual weights of fuel test cups after fuel exposures from zero (initial) to 39 weeks. 86 APPENDIX 31 Exposure time, weeks Pre-paint Postpaint Bare ID 1-1 EG Zn-Ni 1-2 +Cr6 1-3 2-1 EG Zn-Ni 2-2 -Cr6 2-3 3-1 HDGA 3-2 -Cr6 3-3 4-1 HDAℓ 4-2 +Cr6 4-3 5-1 Stainless 5-2 5-3 4 -0.0077 -0.0081 -0.0041 -0.0055 -0.0032 -0.0089 0.0347 0.0329 0.0338 -0.0044 -0.0073 0.0008 -0.0164 -0.0108 -0.0020 8 -0.0026 -0.0047 -0.0018 -0.0023 -0.0024 -0.0047 0.0431 0.0397 0.0421 0.0016 0.0001 0.0064 -0.0130 -0.0071 -0.0026 12 -0.0004 -0.0008 -0.0003 -0.0015 -0.0011 -0.0018 0.0463 0.0401 0.0461 0.0051 0.0017 0.0078 -0.0112 -0.0067 -0.0026 16 0.0018 0.0005 0.0019 -0.0001 0.0007 0.0000 0.0504 0.0446 0.0473 0.0066 0.0040 0.0087 -0.0108 -0.0064 -0.0012 20 0.0014 0.0000 0.0002 -0.0015 -0.0004 -0.0016 0.0499 0.0422 0.0477 0.0041 0.0033 0.0075 -0.0095 -0.0056 -0.0012 24 0.0023 0.0008 0.0004 0.0004 -0.0001 -0.0007 0.0490 0.0446 0.0498 0.0041 0.0034 0.0074 -0.0101 -0.0060 -0.0023 28 0.0027 0.0015 0.0011 0.0007 0.0005 0.0002 0.0543 0.0461 0.0497 0.0044 0.0045 0.0093 -0.0089 -0.0050 -0.0018 32 0.0014 -0.0008 -0.0006 -0.0014 0.0001 0.0003 0.0534 0.0460 0.0484 0.0042 0.0020 0.0070 -0.0094 -0.0057 -0.0024 36 0.0024 0.0014 0.0015 0.0006 0.0007 0.0002 0.0551 0.0478 0.0530 0.0040 0.0036 0.0082 -0.0102 -0.0047 -0.0020 39 0.0053 0.0042 0.0053 0.0047 0.0056 0.0041 0.0607 0.0539 0.0583 0.0081 0.0084 0.0125 -0.0080 -0.0047 -0.0020 6-1 HD Terne 6-2 6-3 7-1 HDSn-Zn 7-2 7-3 8-1 HDAℓ 8-2 8-2 9-1 Fe Stain 9-2 9-3 10-1 304L Stain 10-2 10-3 -0.0016 0.0035 0.0017 0.0015 -0.0022 -0.0021 0.0005 -0.0013 0.0013 0.0012 -0.0028 -0.0002 0.0014 -0.0038 0.0025 0.0025 0.0043 0.0026 0.0017 0.0001 0.0008 0.0012 0.0010 0.0079 0.0027 -0.0008 -0.0007 0.0018 -0.0025 0.0017 0.0045 0.0053 0.0032 0.0014 0.0001 0.0001 0.0008 0.0018 0.0077 0.0038 -0.0010 -0.0004 0.0033 -0.0015 0.0028 0.0049 0.0067 0.0036 0.0030 0.0003 0.0023 0.0020 0.0010 0.0087 0.0003 -0.0005 -0.0009 0.0025 -0.0018 0.0016 0.0061 0.0065 0.0050 0.0035 0.0008 0.0018 0.0023 0.0014 0.0087 0.0028 -0.0015 0.0010 0.0020 -0.0008 0.0020 0.0086 0.0057 0.0057 0.0037 0.0010 0.0024 0.0011 0.0009 0.0089 -0.0001 -0.0007 -0.0001 0.0021 -0.0016 0.0017 0.0152 0.0084 0.0058 0.0036 0.0016 0.0030 0.0018 0.0011 0.0082 0.0009 -0.0016 -0.0002 0.0014 -0.0009 0.0017 0.0166 0.0114 0.0063 0.0042 0.0022 0.0031 0.0013 0.0010 0.0082 0.0014 0.0001 0.0003 0.0010 -0.0015 0.0019 0.0197 0.0138 0.0088 0.0054 0.0032 0.0027 0.0011 0.0010 0.0086 0.0005 0.0001 -0.0008 -0.0002 -0.0020 0.0003 0.0216 0.0167 0.0106 0.0050 0.0035 0.0037 0.0007 0.0001 0.0081 0.0002 -0.0017 -0.0031 0.0013 -0.0013 0.0015 APPENDIX 31. Changes in weight of fuel test cups after fuel exposures from 4 to 39 weeks (positive = weight loss). 87 APPENDIX 32 Exposure time, weeks ID Prepaint Postpaint Bare 1-1 EG Zn-Ni 1-2 +Cr6 1-3 2-1 EG Zn-Ni 2-2 -Cr6 2-3 3-1 HDGA 3-2 -Cr6 3-3 4-1 HDAℓ 4-2 +Cr6 4-3 5-1 Stainless 5-2 5-3 6-1 HD Terne 6-2 6-3 7-1 HDSn-Zn 7-2 7-3 8-1 HDAℓ 8-2 8-3 9-1 Fe Stain 9-2 9-3 10-1 304L Stain 10-2 10-3 INITIAL 33.5038 33.5193 33.4456 34.4235 34.3345 34.1355 28.531 29.1547 29.2427 31.793 31.7794 31.7456 39.4244 39.4167 39.3869 4 33.5035 33.5207 33.4467 34.4206 34.3342 34.1382 28.5086 29.1321 29.2217 31.7817 31.7693 31.7329 39.4262 39.4196 39.388 8 12 16 20 24 28 32 36 39 33.5031 33.5188 33.4453 34.4132 34.3283 34.1312 28.5038 29.1265 29.2154 31.7768 31.7625 31.7281 39.4258 39.4182 39.388 33.5019 33.518 33.444 34.4127 34.3267 34.13 28.5016 29.123 29.2133 31.7761 31.7618 31.7274 39.429 39.4177 39.3871 33.5006 33.516 33.4426 34.4111 34.3251 34.1276 28.4986 29.1208 29.2107 31.7754 31.7605 31.7244 39.425 39.4176 39.3873 33.5015 33.5173 33.4438 34.4116 34.3255 34.1284 28.4989 29.121 29.2109 31.7744 31.7607 31.7247 39.4248 39.4172 39.3872 33.5013 33.5172 33.443 34.4115 34.3259 34.1278 28.498 29.1204 29.211 31.7746 31.7616 31.7255 39.4251 39.4177 39.3879 33.5008 33.5167 33.4422 34.4105 34.3251 34.1273 28.4964 29.1188 29.2074 31.7732 31.7603 31.7236 39.4243 39.4171 39.3872 33.5015 33.5176 33.4431 34.4117 34.3258 34.1285 28.499 29.1219 29.2097 31.776 31.7622 31.7245 39.4246 39.4169 39.3872 33.5009 33.5168 33.4428 34.4113 34.3263 34.1283 28.4974 29.1194 29.2072 31.7742 31.7614 31.725 39.4255 39.418 39.3869 33.4993 33.5149 33.4413 34.4089 34.3234 34.1257 28.4939 29.1163 29.2038 31.7728 31.7592 31.7225 39.4241 39.4166 39.3869 28.7961 28.7135 28.8087 28.9326 29.0179 28.9318 30.8173 30.7306 30.7838 28.5948 28.6853 28.6726 39.0796 38.9533 39.0745 28.7958 28.7125 28.8081 28.9327 29.0174 28.9318 30.8178 30.7313 30.7848 28.5961 28.6863 28.674 39.0784 38.952 39.0738 28.7993 28.7988 28.7983 28.7976 28.7972 28.7973 28.7979 28.7967 28.7972 28.7165 28.7164 28.7159 28.7153 28.7149 28.7146 28.7153 28.7139 28.7138 28.8122 28.8128 28.8124 28.8116 28.8106 28.8105 28.8093 28.8096 28.8088 28.9321 28.9323 28.9322 28.9323 28.9318 28.9325 28.9323 28.9325 28.9325 29.0172 29.018 29.0177 29.0129 29.0171 29.0173 29.0172 29.0174 29.0173 28.9316 28.9323 28.9318 28.9315 28.9314 28.9309 28.9308 28.9314 28.9312 30.8197 30.8192 30.8183 30.8191 30.8177 30.8173 30.8178 30.8176 30.8172 30.7312 30.7317 30.7315 30.7309 30.7308 30.7308 30.7312 30.7309 30.7308 30.7848 30.7861 30.7849 30.7838 30.7846 30.7841 30.7845 30.7842 30.7845 28.5956 28.5962 28.5958 28.5953 28.5955 28.5953 28.5956 28.5956 28.5955 28.6851 28.6864 28.6865 28.6868 28.6857 28.6856 28.6865 28.6867 28.6855 28.6737 28.6743 28.6741 28.6748 28.6736 28.6738 28.6742 28.674 28.6737 39.079 39.0787 39.079 39.0782 39.0782 39.0783 39.0781 39.0784 39.0785 38.9524 38.953 38.9524 38.9525 38.9523 38.952 38.9527 38.9521 38.9522 39.0745 39.0739 39.074 39.0727 39.0738 39.0737 39.0743 39.0735 39.0738 APPENDIX 32. Actual weights of fuel test lids after fuel exposures from zero (initial) to 39 weeks. 88 APPENDIX 33 Exposure time, weeks Pre-paint Postpaint Bare ID 1-1 EG Zn-Ni 1-2 +Cr6 1-3 2-1 EG Zn-Ni 2-2 -Cr6 2-3 3-1 HDGA 3-2 -Cr6 3-3 4-1 HDAℓ 4-2 +Cr6 4-3 5-1 Stainless 5-2 5-3 4 0.0003 -0.0014 -0.0011 0.0029 0.0003 -0.0027 0.0224 0.0226 0.0210 0.0113 0.0101 0.0127 -0.0018 -0.0029 -0.0011 8 0.0007 0.0005 0.0003 0.0103 0.0062 0.0043 0.0272 0.0282 0.0273 0.0162 0.0169 0.0175 -0.0014 -0.0015 -0.0011 12 0.0019 0.0013 0.0016 0.0108 0.0078 0.0055 0.0294 0.0317 0.0294 0.0169 0.0176 0.0182 -0.0046 -0.0010 -0.0002 16 0.0032 0.0033 0.0030 0.0124 0.0094 0.0079 0.0324 0.0339 0.0320 0.0176 0.0189 0.0212 -0.0006 -0.0009 -0.0004 20 0.0023 0.0020 0.0018 0.0119 0.0090 0.0071 0.0321 0.0337 0.0318 0.0186 0.0187 0.0209 -0.0004 -0.0005 -0.0003 24 0.0025 0.0021 0.0026 0.0120 0.0086 0.0077 0.0330 0.0343 0.0317 0.0184 0.0178 0.0201 -0.0007 -0.0010 -0.0010 28 0.0030 0.0026 0.0034 0.0130 0.0094 0.0082 0.0346 0.0359 0.0353 0.0198 0.0191 0.0220 0.0001 -0.0004 -0.0003 32 0.0023 0.0017 0.0025 0.0118 0.0087 0.0070 0.0320 0.0328 0.0330 0.0170 0.0172 0.0211 -0.0002 -0.0002 -0.0003 36 0.0029 0.0025 0.0028 0.0122 0.0082 0.0072 0.0336 0.0353 0.0355 0.0188 0.0180 0.0206 -0.0011 -0.0013 0.0000 39 0.0045 0.0044 0.0043 0.0146 0.0111 0.0098 0.0371 0.0384 0.0389 0.0202 0.0202 0.0231 0.0003 0.0001 0.0000 6-1 HD Terne 0.0005 0.0010 0.0017 0.0021 0.0020 0.0014 0.0026 0.0021 0.0032 6-2 0.0001 0.0006 0.0012 0.0016 0.0019 0.0012 0.0026 0.0027 0.0030 6-3 -0.0006 -0.0002 0.0006 0.0016 0.0017 0.0029 0.0026 0.0034 0.0035 7-1 HDSn-Zn -0.0002 -0.0001 -0.0002 0.0003 -0.0004 -0.0002 -0.0004 -0.0004 -0.0005 7-2 -0.0008 -0.0005 0.0043 0.0001 -0.0001 0.0000 -0.0002 -0.0001 -0.0007 7-3 -0.0007 -0.0002 0.0001 0.0002 0.0007 0.0008 0.0002 0.0004 -0.0002 8-1 HDAℓ 0.0005 0.0014 0.0006 0.0020 0.0024 0.0019 0.0021 0.0025 0.0024 8-2 -0.0005 -0.0003 0.0003 0.0004 0.0004 0.0000 0.0003 0.0004 0.0006 8-3 -0.0013 -0.0001 0.0010 0.0002 0.0007 0.0003 0.0006 0.0003 0.0010 9-1 Fe Stain -0.0006 -0.0002 0.0003 0.0001 0.0003 0.0000 0.0000 0.0001 0.0008 9-2 -0.0013 -0.0014 -0.0017 -0.0006 -0.0005 -0.0014 -0.0016 -0.0004 -0.0002 9-3 -0.0006 -0.0004 -0.0011 0.0001 -0.0001 -0.0005 -0.0003 0.0000 0.0011 10-1 304L Stain 0.0003 0.0000 0.0008 0.0008 0.0007 0.0009 0.0006 0.0005 -0.0006 10-2 -0.0006 0.0000 -0.0001 0.0001 0.0004 -0.0003 0.0003 0.0002 -0.0009 10-3 0.0006 0.0005 0.0018 0.0007 0.0008 0.0002 0.0010 0.0007 0.0000 APPENDIX 33. Changes in weight of fuel test lids after fuel exposures from 4 to 39 weeks (positive = weight loss). 0.0035 0.0040 0.0041 -0.0006 -0.0002 -0.0002 0.0019 -0.0001 0.0000 -0.0005 -0.0012 -0.0003 0.0006 0.0004 0.0007 89 The Strategic Alliance for Steel Fuel Tanks Membership (SASFT): Steel Companies - North America AK Steel Corporation Allegheny Ludlum / Rodney Dofasco Inc. Mittal Steel Company North American Stainless Nucor Corporation Severstal North America Inc. United States Steel Corporation Steel Companies - Europe Arcelor Corus ThyssenKrupp Stahl Steel Companies – Asia JFE Steel Nippon Steel Corporation Nisshin Steel Sumitomo Metal Industries, Ltd. Tata Steel Material/Equipment Suppliers - North America Comau-Pico Harley Davidson Engineering The Magni Group, Inc. Material/Equipment Suppliers - Europe Soudronic Automotive NAFTA Associate Members (Auto Manufacturers) DaimlerChrysler Corporation Ford Motor Company General Motors Corporation Nissan Motor Co., Ltd. Fuel System Manufacturers - North America Elsa LLC Fuel Systems LLC ITT Industries Martinrea International Metalsa Spectra Premium Industries Fuel System Manufacturers - Europe Kautex Textron Inergy Automotive Systems Unipart Eberspacher Fuel System Manufacturers - Asia Dong Hee Industrial Co. Ltd. Horie Metal Co., Ltd. Unipres Corporation Fuel System Manufacturers – South America Aethra Componentes Automotivos For More Information on SASFT: Visit: www.sasft.org Contact: Peter Mould Program Manager 001 810.225.8250 [email protected] For More Information on AISI: Visit: www.autosteel.org Contact: Ronald Krupitzer Senior Director 001 248.945.4761 [email protected] 90