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Effects of Fluoride and Other Halogen Ions on the External Stress Corrosion Cracking of Type 304 Austenitic Stainless Steel

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Effects of Fluoride and Other Halogen Ions on the External Stress Corrosion Cracking of Type 304 Austenitic Stainless Steel NUREG/CR-6539 _ Effects of Fluoride and Other Halogen Ions on the External Stress Corrosion Cracking of Type 304 Austenitic Stainless Steel M low, F. B. Ilutto, Jr. Tutco Scientific Corporation Prepared for U.S. Nuclear Regulatory Commission pfo)D'' ~%, 1 a- ! '% .. lill|Il||# lilllll:[ll[Ill]Ol|Ill E M 72A8A!8 * 7 * CR-6539 R PDR __ . - . .-- I | ! ' AVAILABILITY NOTICE Availabilny of Reference Matenals Cited in NRC Pubhcations Most documents cited in NRC publications will be available from one of the following sources: 1. The NRC Public Document Room, 2120 L Street, NW., Lower Level. Washington, DC 20555-0001 i | 2. The Superintendent of Documents, U.S. Government Pnnting Office, P. O. Box 37082. Washington, DC 20402-9328 l 3. The National Technical information Service Springfield, VA 22161-0002 Although the listing that follows represents the majority of documents cited in NRC publications, it is not in- tended to be exhaustive. Referenced documents available for inspection and copylng for a fee from the NRC Public Document Room include NRC correspondence and internal NRC memoranda; NRC bulletins, circulars, information notices, in- spection and investigation notices; licensee event reports; vendor reports and correspondence; Commissen papers; and applicant and licensee documents and correspondence. The following documents in the NUREG series are aves slo for purchase from the Government Printing Office: formal NRC staff and contractor reports, NRC-sponsored conference proceedings, internatior,al agreement reports, grantee reports, and NRC booklets and brochures. Also available are regulatory guides NRC regula- tions in the Code of Federal Regulations, and Nuclear Regulatory Commission issuances. Documents available from the National Technicallnformation Service include NUREG-series reports and tech - nical reports prepared by other Federal agencies and reports prepared by the Atomic Energy Commission, j' forerunner agency to the Nuclear Regulatory Commission. Documents avsilable from public and special technicallibraries include all open kterature items, such as books, fournal artic.c.% and transactions. Federal Register notices. Federal and State legislation, and congressional | reports can usually be obtained from these libraries. | Uocuments such as theses, dissertations, foreign reports and translations, and non-NRC conference pro- ' ceedings are available for purchase from the organization sponsoring the publication cited. Single copies of NRC draft reports are available free, to tne extent of supply, upon written request to the Office - of Administration, Distribution and Mail Services Section, U.S. Nuclear Regulatory Commission. Washington, DC 20555-0001. Copies of industry codes and standards used in a substantive manner in tho NRC regulatory process are mah- tained at the NRC Library, Two White Filnt North,11545 Rockville Pike, Rockville. MD . 20852-2738 for usa by the public, Codes and standards are usually copyrighted and may be purchased from the originating organiza- tion or, if they are American National Standards, from the American N ational Standards institute,1430 Broad- way, New York, NY 10018-3308. DISCLAIMER NOTICE L This report was prepared as an account of work sponsored by an agcncy of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, expressed or imolied, or assumes any legal liability or responsibility for any third party's use, or the results of such use, of any information, apparatus, product, or process disclosed in this report, or represents that its use by such third party would not infringe privately owned rights. _ ! | _. ._ . _ . _ . ._. _ _ . _ . _ _ . ~ . _ . _ . - _ _ _ . _ _ . _ . _ . _ _ _ . _ _ ; NUREG/CR-6539 | | Effects of Fluoride and Other Halogen Ions on the External | Stress Corrosion Cracking of Type 304 Austenitic Stainless Steel ! | | t i Manuscript Completed: April 1997 Date Published: July 1997 , Prepared by^ K. M. Whorlow, F. B. Hutto, Jr. Tutco Scientific Corporation 676 Peony Drive 4 ' Grand Junction, CO 81503 E. Wco1 ridge,NRC Project Manager Prepared for Division of Engineering Technology Office of Nuclear Regulatory Research U.S. Nuclear Regulatory Commission Wcshington, DC 20555-0001 NRC Jeb Code W6551 | [ ..... __ __ _ _ _ . _ . - _ _ _ _ . _ _ _ _ . _ _ _ . _ . _ _ . _ _ . _ _ . I ! I ' p ABSTRACT ' ' The drip procedure from the " Standard Test Method for Evaluating the influence of Thermal- Insulation on External Stress Corrosion Cracking Tendency of Austenitic Stainless Steel"(ASTM | .C 692-95a) was used to research the effect of halogens and inhibitors on the External Stress Corrosion Cracking'(ESCC) of Type 304 stainless steel as it applies to Nuclear Regulatory ; ' ! Commission Regulatory Guide 1.36.'" Nonmetallic Thermal Insulation for Austenitic Stainless | Steel." The solutions used in this research were prepared using pure chemical reagents to simulate . the halogens and inhibitors found in insulation extraction solutions. The results indicated that sodium silicate compounds that were higher in sodium were more effective for preventing chloride-induced ESCC in type 304 austenitic stainless steel. Potassium silicate (all- > silicate inhibitor) was not as effective as sodium silicate.' Limited testing with sodium hydroxide : (all-sodium inhibitor) indicated that it may be effective as an inhibitor. ,! Fluoride, bromide, and iodide caused minimal ESCC which could be effectively inhibited by sodium * silicate . The addition of fluoride to the chloride / sodium silicate systems at the threshold of ESCC | appeared to have no synergistic effect on ESCC. The mass ratio of sodium + silicate (mg/kg) to chloride (mg/kg) at the lower end of the NRC RG 1.36 Acceptability Curve was not sufficient to prevent ESCC using the methods of this research. ! i : ' | , i l | | .j l' ; ' | ! I t- |~ , ! I i I , I iii NUREG/CR-6539 i . .. - .- 1 CONTEETS 4 Page . ABSTRACT iii | L INTRODUCTION 1 ' BACKGROUND 1 External Stress Corrosion Cracking 1 History of ESCC Test Procedures 1 Stainless Steels 2 Corrodants and Inhibitors 2 Acceptance Criteria. 3 ~ TEST PROCEDURES 4 ASTM C 692-95a 4 Metil Certification Data 4 TEST PROGRAM 5 Test Solutions 5 Evaluation 6 RESULTS 7 Metal Qualification With Deionized (DI) Water 7 Inhibitor Program (Identifying the Threshold-Chloride Pass) 7 Synergistic Effect of Fluoride on the Action of Chloride 7 Long-Term Tests 8 Combination Fluoride, Bromide, Iodide 8 28-Day Fluoride Tests 8 Fluoride Inhibition 8 Bromide and Iodide Inhibition 8 DISCUSSION ' 9 Inhibitor Program Results vs. NRC RG 1.36 Acceptability Curve 9 Mole Ratio 9 Fluoride as an ESCC Promoter 10 Verification Tests and Fiuoride Addition to Threshold Passes 10 Combination Fluoride, Bromide, and Iodide 11 Bromide and Iodide 11 . ; v NUREG/CR-6539 |' -- , CONTENTS _(santianed) Page CONCLUSIONS ii REFEllENCES 12 APPENDIX A (Tables 1-10) 13 APP 8NDIX B (Figures 1-12) 25 IM AGES (1-6) 38 | | | | ) NUREG/CR-6539 vi | - _ _ - - _ - _ - _ _ _ _ - _ _ _ _ \- .s Acknowledgments This work was supported by the Office of Niiclear Regulatory Research in the U.S. Nuclear Regulatory Commission (NRC), under Contract No. NRC-04-96-038 with Modification , 1. The authors are grateful to Program Manager, Edward O. Woolridge, for his technical input, ) guidance, and recommendations during the course of the project. n' , ) vii NUREG/CR-6539 t _ _ - - - _ _ - . _ . i ! ! INTRODUCTION The purpose of this research was to provide to the Nuclear Regulatory Commission new information | , | on the effect of chloride, fluoride, bromide, and iodide on ESCC of type 304 austenitic stainless ! steel, and to determine the role of sodium + silicate as an effective inhibitor for ESCC induced by | these ions. The drip test methodology of ASTM C 692-95a (Standard Test Method for Evaluating the Influence of Thermal Insulations on External Stress Corrosion Cracking Tendency of Austenitic Stainless Steel) was used for this study. The topics addressed included : 1) the effect of the molar ratio of sodium-to-silicate in the inhibitor; 2) the amount of sodium + silicate necessary to inhibit the ESCC action for specific amounts of chloride (mass ratioh 3) the presence or absence of a syner- gistic effect of fluoride on the action of chloride: 4) the possibility for ESCC induced by fluoride, bromide, and iodide ions, and if found, its inhibition by sodium + silicate, BACKGROUND External Stress CorrosloILCmC}Jng ESCC is a type of corrosion involving cracking that occurs on the outside surface of thermally- insulated pipes or vessels and is often associated with austenitic stainless steels. For ESCC to take place several factors are usually present: tensile stress, moisture, heat, an aggressive chemical environment, and sensitized metal. Heat-treatment or welding sensitizes the metal by depleting the chromium in the grains and forming chromium compounds at the grain boundaries. ESCC ofinsulated pipes became recognized as a serious problem in the 1950's[1], and researchers in the industry quickly devised methods for pre-qualifying insulating materials for use in contact with austenitic stainless steel. Several specifications were promulgated in the sixties and seventies but only two remain: ASTM C 795 (Standard Specification for Thermal Insulation for Use in Contact with Austenitic Stainless Steel) and MIL-1-24244 (Insulation Material, with Special Corrosion, Chloride, and Fluoride Requirements). Regulatory Guide 1.36 (Nonmetallic Thermal Insulation for Austenitic Stainless Steel) was issued in 1973 and, while not a specification or a regulation, RG 1.36 suggests the use of the ASTM and / or RDT test procedures to qualify insulation for use in nuclear facilities. The ASTM and MIL-1 specifications have been periodically updated. The RDT procedures are outdated and have been abandoned (see 3d paragraph under " History "). The Nuclear Regulatory Commission, in their - efforts to revise RG 1.36, required additional information as noted in items 1 - 4 of the Introduction. History of ESCC Test Procedures in the early 1950s, tb test method that has become known as the Dana test originated in the DuPont laboratories.
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