ML20058F672

TMI-2 Intrument Nozzle Exams at Argonne Natl Lab

ML20058F672
Person / Time
Site:	Crane
Issue date:	02/28/1993
From:	Hins A, Neimark L, Purohit A, Shearer T ARGONNE NATIONAL LABORATORY
To:	NRC
Shared Package
ML20058F640	List: ML20058F639 ML20058F643 ML20058F648 ML20058F656 ML20058F663 ML20058F672 ML20058F679 ML20058F691
References
TMIV(93)AL01, TMIV(93)AL1, NUDOCS 9312080223
Download: ML20058F672 (100)

Text

{{#Wiki_filter:l TMIV(93)ALO1 j u Q"R "L OECD-N EA-TMI-2 C' s Vessel Investigation Project Il [ v, m. %'ii M4SC TMI-2 Instrument Nozzle (* r = Examinations at Argonne li National Laboratory _2_ ^ O - L. A. Neimark, T. L. Shearer, A. Purchit, and A. G. Hins February 1993 i 3 i l NOTICE This report is for the benefit of OECD TMI i participants and their designees only i This report has been prepared pursuant ts. OECD agreements on the TMI 1 Vessel investigation Project. ? Is the policy that the Information contained in this report be c.ed only for the benefit of the participants and the participai.t3 designees. The contents of this report should not be disdosed to others or reproduced wholly or partially unless authortred in accordance with the laws, regulations, policies, or written permission of the appropriate project participant. 9312080223 931126 .4 DR ADocK 0500 0.

9

,i yy. )

x The contents of this report were deueloped as part of the Three Mile Island Unit 2 Vessel Investigation Project. This project is jointly sponsored - by eleven countries under the auspices of the Nuclear Energy Agency of the Organisation for Economic Cooperation and Development. The eleven sponsoring organisations are: The Centre d' Etudes d'Energie Nucidaires of Belgium, The Sateilyturvakeskus of Finland, The commissariat a l'Energie Atomique of France, The Gesellschaft f0r Reaktorsicherheit mbH of Germany, l The Comitato Nazionale per La Ricerca e per lo Sviluppo Dell' Energia Nucleare e Delle Energie Alternative of Italy, 1 The Japan Atomic Energy Research Institute, The Consejo de Seguridad Nuclear of Spain, The Statens K&rnkraftinspektion of Sweden, The Office F6dsral de l'Energie of Switzerland, AEA Technology of the United Kingdom and The United States Nuclear Regulatory Commission. l The primary objectives of the Nuclear Energy Agency (NEA) are to promote cooperation between its Member governments on the safety t.nd regulatory aspects of nuclear development, and on assessing the future role of nuclear energy as a contributor to economic progress. This is achieved by: - encouraging harmonisation of governments' regulatory policies and practices in the nuclear field, with particular reference to the safety of nuclear installations, protection of man against ionising radiation and preservation of the environment, radioactive waste 4 l management, and nuclear third party liability and insurance; - keeping under review the technical and economic characteristics of nuclear power growth and of the nuclear fuel cycle, and assessing I demand and supply for the different phases of the nuclear fuel cycle i and the potential future contribution of nuclear power to overall energy demand; I - developing exchanges of scientific and technical information on nuclear energy, particularly through participation in common services; J - setting up international research and develcoment programmes and undertakings jointly organised and operated by OECD countries. In these and related tasks, NEA works in close collaboration with the International Atomic Energy Agency in Vienna, with which it has concluded a ( Cooperation Agreement, as well as with other international organisations in i the nuclear field. } i r

TMIV(93)AL01 .i I l l TMI-2 INSTRUMENT N0ZZLE EXAMINATIONS AT ARGONNE NATIONAL LABORATORY by l l L. A. Neimark. T. L. Shearer. A. Purohit, and A. G. Hins l t February 1993 I l i Materials and Components Technology Division Argonne National Laboratory ~ Argonne. IL 60439 l Prepared for the j OECD-NEA-TMI-2 q Vessel Investigation Project i Work Sponsored by the U.S. Nuclear Regulatory Commission under an Agreement with the U.S. Department of Energy

i Contract W-31-109-Eng-38

-l a

't t I i i i TABLE OF CONTENTS i Pace ABSTRACT.................................................................. vi I. INTRODUCTION........................................................ 1-11. 0BJECTIVES.......................................................... 2 111. SC0PE............................................................... 3 3 IV. GENERAL PROCEDURES.................................................. 3 V. EXAMINATION RESULTS................................................. 5 A. Nozzle M9....................................................... 7 i B. NozzleL6...................................................... 1'O f C. Nozzle H5................................... 12 D. Nozzle H8............. 15 i E. Nozzle D10.................. 17 F. Nozzle E11...................................................... 22 VI. DISCUSS 10N.......................................................... 25 i A. Defining " Debris"............................................... 25 -l B. Nature of Nozzle Damage......................................... '26 ] C. Postulated Fuel Relocation Scenario............................. 28 j D. Presence of Control Assembly Materials.......................... 31 l E. Temperature Indicators.......................................... 33 i f F. Penetration of Materials into Nozzles............................ '35 Vll. CONCLUS10NS......................................................... 37 a 1 Vill. ACKNOWLEDGMENTS..................................................... 38 i IX. REFERENCES............-............................................. 39 l X. APPENDIX.. '102 i J e 1 ) ) s l i .}

l I i' LIST OF FIGURES Pace 1. Grid map of TMI core showing locations of nozzles examined at ANL..... 44 l 2. Typical in-core nozzle with seal and retaining weld................... 45 3. Lower head area and in-core instrument guide tubes............ 46 i 4. El evation view of nozzl e segment M9. a s received...................... 47 5. Top and bottom views of M9 nozzle segment. as received............... 48 -f 6. Gamma activity profile and sectioning scheme for Nozzle M9............ 49_ 7. Longitudinal sections through top of Nozzle M9 near the center (left) and at the center (right)...................................... 50-l 8. Longitudinal section through top of Nozzle M9......................... 51 9. SEM-BSE image of multiphase fuel in Nozzle M9......................... .52 10. As-cut transverse section at 241-mm elevation of M9. showing t i metallic and possibly ceramic debris between 5 and 8 o' clock in the annulus........ 52' i i 11. Elevation view of nozzle segment L6................................... 53 l r 12 Top and bottom views of L6 nozzle segment............................ 54 .13. Gamma activity profile and sectioning scheme for Nozzle L6............ 55 j s 14. As-cut transverse section at 283-mm elevation of L6. showing a .i i porous material in the annulus......... 56- [ 15. Instrument string and fuel debris at 283-mm elevation of L6........... 57 i i 16. Partially transformed fuel mass at 283-mm elevation of L6............. 58 17. As-cut transverse section at 77-mm elevation of L6.................... 58- .i r r 18. Partially transformed zirconium instrument lead at 77-mm elevation 7 in L6.............. 59 t h ? ll t

s f i 19. Etched microstructure of Incor.el 600 nozzle at 77-mm elevation in j L6.................................................................... 59 I 20. Elevation view of nozzle segment H5................................... 60 ? 21. Top and bottom views of H5 nozzle segment............................. 61' j i 22. As-polished bottom end of H5 segment, revealing ~only a solidified metallic mass......................................................... 62 23. Gamma activity profile and sectioning scheme for Nozzle H5............ 63 j 24. As-cut transverse section through H5 at the 114-mm elevation.......... 64 25. As-cut longitudinal section through top of H5 segment................. 64 i 26. Metallic and ceramic debris at top of Nozzle H5....................... 65 -i i 27. Microstructure of debris at top of Nozzle H5. showing intimate mixture of U-rich phases (light). Zr-rich phases (medium), and l i Cr-rich matrix (darkest).............................................. 66 j 28. Chromium-rich platelets precipitated in Cr-depleted Inconel...... 66 29. Instrument string and solidified Inconel mass at the bottom of j the H5 segment........................................................ 67 l l 1 30. Shards of Inconel 600 (a) and fuel debris (b) within instrument 1 i string at bottom of H5................................................ 68 1 31. Bottom weldment of the H5 nozzle........................................ 69. 32. Top, elevation, and bottom views of H8 nozzle segment..... 70 33. Gamma activity profile and sectioning scheme for Nozzle H8............ 71 34. As-cut longitudinal section.through the top of H8............ 72 35. As-cut transverse section at the 64-mm elevation in H8..........-...... 73 36. Metallographic'section of instrument string and metallic debris at the 64-mm elevation of H8............... 74 in i

j l .37. Eutectic structures containing Zr U In, Ni, Cr, and Fe. at the 64-mm elevation in H8................................................. 75 i 38. Ablated surface of H8 nozzle at the 64-mm elevation............... 76 39. SEM-BSE image of Ag-Cd particle, and Zr-rich material penetrating l surface of H8 nozzle at 64-mm elevation............................... 76 40. Elevation views of DIO nozzle segment................................. 77 i 41. Top and bottom views of the DIO nozzle segment........................ 78 j I 42. Gamma activity profile and sectioning scheme.for DIO nozzle segment... 79 'l I 43. Two sides of the longitudinal section through the top of the j D10 nozzle............................................................ 80 { 44. Typical area of fuel snards found at top of J10 nozzle....... 81 I 45. As-cut transverse section through D10 at the 266-mm elevation, showing metallic and ceramic debris inside............................ 81 46. Surface deposits at 266 mm ca Nozzle D10.............................. 82 2 I 47. As-cut transverse section through DIO at the 177-mm elevation......... 82 e i i 48. AS-cut transverse section through DIO at the 158-mm elevation......... 83 j i 49. Area of grain bou'.dary separations in D10 at the 158-mm elevation..... 84 j 1 i 50. Examples of Ag-Cd deposits in D10 at the 158-mm elevation, showing f e Ag-Cd penetration as (a) stringers and (b) discrete particles......... 85 51. Examples of particulate fuel debris trapped in grain boundary' i separations at 158 mm in D10.......................................... 86 i -{ a. I 52. Area of grain boundary separations in DIO at the 158-mm elevation. [ etched to show possible second phase and internal grain. structure...., 87 l 53. Portion of thick exterior deposit on D10 at the 158-mm elevation...... 88 { 54. Examples of Ag-Cd in inconel at 158-mm in Nozzle D10.................. 89 t e i IV 9

t 55. Segregated U-rich (light) and Zr-rich (dark) phases in fuel particle in a deposit at 158 mm on D10................................. 90 56. Instrument string at 158 mm in D10.................................... 91 57. Mel ted Z r l e a d wi re a t 158 mm i n D10.................................. 92 58. Layer of debris on outer surface of D10 at the 82-mm elevation........ 93 59. Elevation view of nozzle segment E11.................................. 94 60. Top and bottom views of nozzle segment E11............................ 95 61. Gamma activity profile and sectioning scheme for Nozzle E11........... 96 62. As-cut transverse section at 274 mm and longitudinal section through top of Nozzle E11................................... 97 63. Fuel debri s i n the top of Nozzl e E11................................... 98 64. " Micro-folds" with trapped fuel debris in the outer surface at the top of Nozzle E11................................................. 99 65. SEM image of fuel debris attached to the inner surface of Ell at the 274-mm elevation.. 99 66. SEM image of surface reaction at 274 mm on E11........................ 100 67 As-cut transverse section through E11 at 220 mm........................ 100 68. Flaking surface debris-bearing scale and surface-adherent scale beneath it at 90-mm elevation on Nozzle E11........................... 101 69. SEM-BSE image of scales shown in Fig. 68.................... 101 LIST OF TABLES 1. ANL Nozzle Segment lengths. Elevations, and fuel Penetration Depths... 40 2. Composi tion of Debri s Area s/Pa rti cles Containing U-Zr................. 41 3. Summary of Hardress Determinations.................................. 43 v

j i 4 j ABSTRACT l i e i Six of the fourteen instrument tube nozzles extracted from the TMI-2 lower j j j head were examined at Argonne National Laboratory to provide information on f their metallurgical state, on interactions with core debris that made its way f 3 to the lower head, and on penetration of the core debris into the nozzles. [ The objectives of the examinations were to determine the temperatures near the l t lower head, the mechanisms, modes, and extent of nozzle degradation to evalu- ? 4 ate the challenge to the lower head containment boundary, and contribute to i the generation of a scenario for fuel movement on the lower head. The exami-nation techniques were visual examination, gamma scanning, metallography, mi-crohardness measurements, and scanning electron microscopy-energy dispersive ? X-ray (SEM-EDX) analysis. t I j The results of the examinations indicate that some nozzles were melted off ( r } by interaction with molten core debris, whereas others were only thermally f affected by contact with core debris, some of which attached itself to nozzle l surfaces. The elevations at which the nozzles were melted off suggest that i j the liquid core debris was atop c crust of solidified material that apparently l generally insulated the reactor vessel from the Sottest debris. The pattern j of nozzle degradation was consistent with the location of a hot spot in the 4 vessel at the C7-8/F7-8 location as determined by metallurgical examination of i the vessel steel samples by others. Based on the severe damage to some noz-j zles and not to others in relatively close proximity, it can be concluded that .f f the flow of material across the lower head was multi-directional and not ' uni-3 j fied. It is believed that a significant portion of the core debris moved i ] across the lower head, from the east and southeast toward the hot spot, in a f 1 0 t lava-like flow, the basal crust insulating the vessel and the lower portions i 3 ef the nozzles. The finding of significant quantities of control assembly ma-terials (Ag, Cd, In, Ir, Fe, and Cr without U) in the nozzle material and on nozzle surfaces indicates their presence on the lower head prior to the mas-l l sive relocation of core debris 226 minutes into the accident. I i I l

TMI-2 INSTRUMENT N0ZZLE EXAMINATIONS AT ARGONNE NATIONAL LABORATORY by L. A. Neimark T. L. Shearer, A. Purohit, and A. G. Hins 1. INTRODUCTION The accident at the Three Mile Island Unit 2 (TMI-2) reactor in March-1979 resulted in the relocation of approximately 19.000 kg of molten core ma-terial to the lower head of the reactor vessel.1 This material caused exten-sive damage to the instrument guide tubes and nozzles and was suspected of having caused significant metallurgical changes in the condition of the lower head itself. These changes and their effect on the margin-to-failure of the lower head became the focal point of an investigation co-sponsored by the United States Nuclear Regulatory Comnission (NRC) and the Organisation for Economic Co-operation and Development (DECD). The TMI-2 Vessel Investigation Project (VIP) was formed to determine the metallurgical state of the vessel at the lower head and to assess the margin-to-failure of the vessel under the conditions existing during the accident. Under the auspices of the VIP. specimens of the reactor vessel were re-moved in February 1990 by MPR Associates. Inc.2 In addition to these speci-mens, fourteen ir.strument nozzle segments and two segments. of instrument guide tubes were retrieved for metallurgical evaluation. The purpose of this'evalu-ation was to provide additional information on the thermal conditions on the lower head that would influence the margin-to-failure, and to provide insight into the prcgression of the accident scenario, specifically the movement of the molten fuel across the lower head. ( 1

. ~ [ 't t t .II. OBJECTIVES j i The VIP has as its principal goal the determination of the margin-to-failure of the reactor's lower head. Concomitant with this goal is the devel-opment of a lower-head-damage scenario and input data needs for the margin-to-failure analysis. To this end, the Idaho National Engineering Laboratory (INEL) developed a VIP Coordination Plan that identifies the scope of the lower-head-damage-scenario needs and the data required for the margin-to-fail-r ure analysis. Thus, the overall objectives of the nozzle examination effort at Argonne National Laboratory (ANL) were to f (1) Provide information on the temporal and locational movement of fuel onto and across the lower head; l (2) Estimate peak temperatures of the nozzles from their metallurgical end-state; and 4 (3) Determine the mechanisms, modes, and extent of nozzle degradation to evaluate the imperilment of the lower-head containment bound-1 ary. i Data requirements provided in the Coordination Plan established the fol-lowing specific objectives for the nozzle examinations: l \\ 1 l I (1) Determine the nature and extent (axial and radial) of fuel / debris ingress into a nozzle: .j .I l (2) Determine the nature and degree of chemical and thermal interac-tion between fuel, debris, and nozzles: 4 (3) Determine thermal-related metallurgical changes in the nozzle as a function of axial position to evaluate the axial temperature dis-tribution and attempt to quantify temperatures near the vessel:- and ] 2 1

(4) Determine the position and composition of debris adhering to noz-zie surfaces to establish a " debris bed depth". In addition to satisfying the contribution of ANL to the data needs, an evaluation of the data obtained would be a good basis for contributing to an accident scenario that describes the fuel movement across the lower head. I 111. SCOPE Fourteen nozzles were removed from the TMI-2 lower head. Six of these were examined at ANL and eight were to be examined at INEL. l The scope of the examinations at ANL consisted of visual examination and macrophotography, axial gamma scanning (137Cs). Sectioning followed by macro-I photography of the as-cut surfaces, metallogr3phy with selected microphotogra-phy (some in the etched condition). microhardness measurements on selected samples, and scanning electron microscopy-energy dispersive X-ray (SEM-EDX) l analysis on selected samples. In all. 43 samples were prepared metallo-graphically. This seemingly large number was required because the metallo-graph stage limited the mount size to a diameter of 32 mm. Of these. 33 sam-pies were examined by SEM-EDX. the microhardness was measured on 21. and three were etched to observe the microstructure. IV. LENERAL PROCEDURES The nozzles were received in individual sealed containers. Each was vi-sually examined immediately after removal from its container to identify any especially notable areas. Macrophotography was done at IX magnification through a hot-cell window with a long-bellows camera. Photos were taken of the entire external surf ace at 120* intervals, of the bottom surf ace, as cut .t TMI. and of the top surf ace. Sometimes in stereo because of the complex, three-dimensional nature of the surface. for gamma-scanning. each nozzle was placed in an aluminum container to prevent loss of material that might slough off. Scanning along the height of the nozzle was performed as the container was slowly moved across the face of 3

a collimated germanium detector. Only 137Cs activity was scanned because this would be representative of the UO2 fuel. The locations on each nozzle to be sectioned for further investigation were established based on a combination of the following criteria: (1) Top and bottom locations to obtain information on the hottest (sometimes molten) and coldest (nearest the vessel) temperature extremes in a nozzle: (2) Fuel / nozzle interaction areas (nozzle degradation mechanism): (3) Indications from gamma scans of fuel penetration into the nozzle: (4) Obvious locations of surface layers on a nozzle: and (5) Locations of surface cracking (nozzle degradation mechanism). Before sectioning, each nozzle was placed in a copper tube, 6.35 mm in 1 diameter, which was then vacuum-impregnated with cold-setting epoxy resin. This was done to stabilize loose surface debris, fragile solidified masses, and internal components. Additional vacuum-impregnation was done during sec-tioning if significant voids were found in the epoxy and there was a possibil-ity of material fall-out. l Transverse sectioning was done with a dry sic cut-off wheel while the canned nozzle was rotated in a chuck. The cutting, therefore, was actually circumferential to eliminate localized heeting. Longitudinal sections cere made with a reciprocating motion of the blade. The location of the longitudi-nal cuts in the sectioning diagrams in this report are not shown in the actual plane of cutting because it is not possible to do this in an elevation view. The locations provided are intended to indicate only the degree of segmenta-tion of each nozzle. Metallographic specimens were placed in hollowed-out, preformed Bakelite mounts. vacuum-impregnated with epoxy resin, and polished with diamond paste down to 1 p using a kerosene-based lubricant. 4

Microhardness was measured with a diamond pyramid indentor in a Leitz MMS-RT metallograph and a 200-9 load. Usually, five to ten measurements were made, from the nozzle surface (inner or outer) inward. Values affected by the surface or internal voids were rejected, Although a surface hardening, or a subsequent softening attributed to accident-induced annealing, could be dis-cerned in some measurement profiles, for purposes of this determination, the population was averaged and a standard deviation reported. This data treat-4 ment appears to be adequate to identify qualitative trends in the axial tem-perature distributions of the nozzles and provide some insight into quantita-tive temperatures when compared to limited data from Korth.3 Some very low measured values proved to be from areas that were either once-molten, had been involved in liquid-metal attack, or were depleted in Cr and thus no longer Inconel 600. These low values are not representative of a metallurgical state of the Inconel 600 that could be used as a temperature indicator. Because the Project has not been able to determine a correlation between microhardness and the metallurgical state of true archival Inconel 600 nozzle material, the mi-crohardness data are, at best, qualitative. A number of etchants for Inconel 600 were tried, but 3 pts glycerine-3 pts hcl-1 pt HNO3 gave the best results. However, because of the lack of com-parative microstructures of archival material that could be used in a time / l temperature effect correlation, the effort to etch more samples was abandoned. V. EYAMINATION PESULTS This section will describe the examinatien results on a nozzle-by-nozzle basis, moving essentially from east to west along the lower head. It is be-lieved tnat this was the direction of the principal fuel flow across the lower head some 226 minutes into the accident. l The six nozzles examined at ANL were f rom core locations M9, L6, H5, H8, 1 l D10. and Ell; their locations on the reactor grid are shown in Fig. 1. The damage to these nozzles provides a representative sample of the damage that I occurred to all 14 nozzles that were removed f rom the vessel and, together 1 with information from the eight nozzles being examined at INEL, provides good 5

information from which to construct a scenario for the temporal and locational movement of molten fuel onto and across the lower head. The typical. nozzle configuration is shown in Fig. 2. -l In the course of analyzing the results for the preparation of this re-port, it was discovered that four of the six ANL nozzles had been mis-identi-fied during the handling process before the nozzles arrived at ANL. The basis for subsequently making the true identification of these nozzles was a compar-ison of the records generated by MPR Associates 4 and the. visual observations made when the nozzles arrived at ANL. The mis-identified nozzles were HS (nee D10). DIO (nee H5). Ell (nee L6), and L6 (nee Ell). All nozzle identities in' this report are the true identities, except any references, as above, to the former identity. It must be recognized that these identities differ from those in all previous presentations of ANL's nozzle examination results. The true nozzle identities now provide a more consistent story of the conditions-on the lower head than previously conceived. To provide the reader with a perspective of the cbserved damage to indi-vidual nozzles with respect to a global lower-head-damage scenario, two sample elevations are used in this report where appropriate. The primary sample ele-vation is the distance from the base of the nozzle, which was not usually the cut-off surface during removal from the vessel. The second elevation is the vertical distance from the lowest vessel location, at H8 (Fig. 1), to the noz-zie surface in question. Figure 3 shows the relationship of these reference elevations. The severing of the nozzles from the vessel usually left a stub attached to the vessel. The height of this stub for the ANL nozzles was de-termined either from the nozzle's companion boat sample that was processed at ANL, or from knowledge of the nozzle's dimensions, as shown in Fig. 2. fer Nozzles M9 and L6, there were no companion boat samples, and the latter method was used. Thus, the reported sample elevation for a given nozzle is the height of the residual stub plus the distance on the nozzle from the cut-off end to the particular elevation. The secondary elevation is the primary eie-vation plus the elevation from the low-point reference (location H8) to the base of the particular nozzle. (NOTE: In previous ANL reporting and presen-tations, the " elevation" has been only the distance on the nozzle from the 6

i cut-off end to the particular elevation. The changes have been made to better reflect the elevation of a location for debris penetration and axial tempera-ture considerations and for accident scenario considerations.) Table 1 pro-vides a summary of nozzle segment lengths and relevant elevations. Also tabulated in Table 1 are the fuel penetration distances into each nozzle, as determined by the 137Cs axial activity profile. The data are pro-vided as the elevation of fuel material above the base of the nozzle. Maximum and minimum values are given for nozzles for which it could not be absolutely 137 s activity was inside and not on the surface of the noz-C concluded that the zle. The use of the gamma-activity profiles rather than visual observation of " ceramic" material in the nozzle cavity was deemed more appropriate because of the possibility that the ceramic" material could be a nozzle oxidation prod-uct and not actually a fuel mass. A. Nozzle M9 The M9 nozzle segment received at ANL was 254 mm long. Based on a nomi-nal as-fabricated nozzle length of 305 mm (centerline: slope of base not con-sidered), a 26-mm stub remained on the vessel after severance. Figure 4 shows ~ one view of Nozzle M9 as it was received. The top 25 mm of the nozzle had been melted off and the next 25 mm show signs of melting, including the initi-ation of "andling. The 25-50 mm below the melted area appeared to be lightly scaled, whereas the remainder of the nozzle was bright and shiny. As-fabri-cated vibra-tooled lettering was apparent just below the midplane. Figure 5 shows the top and bottom views of the as-received nozzle. The top appeared to be totally sealed with molten material, whereas the bottom showed no material in the annulus between the instrument string and the noz-zie; however, there appeared to be material in the central tube of the instru-ment string. The axial gamma scan and the locations of major cutting of the nozzle with the resulting breakoff identifications [ Alpha / Gamma (A/G) hot-cell num-bers] are shown in Fig. 6. The A/G numbers correspond to the specimen identi-fications found in the Appendix. This sectioning provided an overall view of 7

the damage to the top of the nozzle where the gamma scan indicated the pres-ence of fuel, and an area from the bottom of the nozzle where core debris may have been in intimate contact with the outer surface.1 Figure 7 shows two as-cut longitudinal surfaces through the top of the nozzle. Melting of the noz-zie was restricted to the top 25 mm, but the instrument tube showed signs of melting below that elevation. Vertically-oriented voids in the molten nozzle were also found in other ance-molten nozzles. The voids are believed to be the result of a solidification phenomena in which spherical voids interlink in a vertical array and surface tension causes the horizontal ligaments to con-tract and disappear, and thus form a continuous longitudinal void. Such spherical voids, or bubbles, are shown in the molten material in Fig. 8. The spherical bubbles, which were closer to the nozzle centerline, would be indic-ative of rapid cooling, whereas the longitudinal bubbles outward from the cen-ter would be indicative of a somewhat slower cooling rate. In Fig. 8, the metallic debris in the center (bright phases) is the remnant of the outer tube of the instrument string (Inconel 600), whereas the gray phases are, appar-ently, Oxides of the metal and fuel (the SEM-EDX system cannot analyze for oxygen). What remains of the instrument leads (generally Zr wires in Al 03 insula-2 tion with Ince-sheathing) is on the right in Fig. 8. The gray mass on the left, adjacent to the molten nozzle, is Cr-rich, apparently an oxide. The adjacent molten Inconel was almost devoid of Cr. The lighter ceramic phases surrounding the metallic phases in the center consisted of discrete areas of fuel of different macro-compositions and void morphologies. The macro-compo-Sitions of these areas are given in Table 2., which summarizes the compositions and locations of selected fuel-bearing species that were identified during ex-amination of the nozzles. The general matrix in which these discrete fuel islands exist is essentially a solidified Cr-oxide which contains fine bits of solidified fuel as a "second phase." On a microscopic scale, some of these areas, shown in Fig. 9. consisted of Zr-rich phases with significant U con-tent. U-rich phases with significant Zr content, and Cr-rich areas with traces of Fe, Ni, Ti, Mn, Zr. and U. The segregation into U-rich and Zr-rich fuel phases is indicative of a sufficiently slow cooling rate for segregation to occur. The spherical bubbles contained apparently condensed phases of Al, Si, 8

and Ca while other bubbles contained Ag and Cd deposits. The presence of Ag-Cd in the molten Inconel indicates that these materials were either in or on the nozzle at this location before melting occurred. A transverse section 38 mm below the top of the melted-off nozzle in the scaled area (241 mm from the base) is shown in Fig. 10. This section shows a metallic mass that is similar in appearance to a mass in the H8 nozzle that analysis showed to be molten Inconel 600, but deficient in Cr. On the basis of that similarity, no metallography or SEM work was undertaken for this sec-tion. A possible ceramic mass, which could be fuel, is also visible in Fig. 10. Fuel is a distinct possibility because this area is at the lower end of the 137Cs activity profile shown in Fig. 6. A segment of the nozzle surface 38 mm above the base (183 mm above the lowest point in the vessel), from the very clean area in Fig. 4, was examined by SEM-EDX to search for evidence of debris deposits. A 0.5-1.0- -thick layer of enhanced Cr material, apparently Cr-oxide, was found on the surf ace, along with occasional deposits of Al, probably Al 0. There were traces of control 23 rod materials in the Cr-oxide layer, but no fuel. Also, there was no Fe-ma-trix layer that contained core debris. The principal gamma activity peak at the top of the nozzle (Fig. 6) cor-responds to the fuel that was found at this location. The secondary peaks are adjacent to the scaled surface area, which was not found to contain measurable quantities of fuel in the area examined. These peaks likely reflect fuel in the outside candling piece and/or fuel in the inside candling material. For purposes of a debris penetration distance, the 241-mm elevation is suggested as at least a minimum, as indicated in Fig.10. Microhardness measurements were made on a specimen from the top longitu-dinal section and on the bottom nozzle specimen. The measurements at the top averaged 124 2 5 diamond-point hardness (DPH), while the average of measure-ments from the bottom specimen was 202 28 DPH. A summary of all hardness measurements on all nozzles is given in Table 3. The low values from the top 9 __..__________..m_

reflect the significant Cr depletion in this area, with the result that the matrix was no longer Inconel 600. B. Nozzle L6 The L6 nozzle segment (nee Ell) was -241 mm long, and a stub -64 mm high would have been left on the vessel. Figure 11 shows one view of the nozzle as it was received. This nozzle was essentially untouched externally by the ac-cident. Vibra-tooled identification markings are clearly visible on the non-scaled surface. The four notches in the side of the nozzle were put there by MPR Associates for identification purposes. The top and bottom views, Fig. 12, show that the instrument string was either snipped off or bent off, but not melted off. Debris inside the nozzle, external to the instrument string, can be seen in both the top and bottom views. The 137Cs axial gamma Fig. 13, indicates that the contained material is apparently fuel-

scan, bearing.

The nozzle was sectioned transversely at five locations as shown in Fig. 13. These elevations were selected principally to attempt to determine 137 s activity inside the noz-C the nature of the material that was Creating the zle. Figure 14 shows an as-cut section 22 mm below the top of the nozzle (283-mm elevation), and a gray, porous ceramic-appearing material. Some of the fuel in the top of the nozzle can be seen in Fig. 15: the rest was appar-ently lost in the cutting operations. Analysis of the fueled areas showed a potpourri of materials and compositions. The triangular particle in Fig.15 was pure UO, apparently unmelted and a true pellet fragment. The porous mass 2 at 3 o' clock in this figure contained U, Zr, Fe, Cr, and Al. The microstruc-ture of this particle Fig.16. shows that the fuel had been only partially transformed into U-rich (light) and Zr-rich (medium) phases, indicating rapid cooling. The Fe. Cr, and Al are the dark phase in the grain boundaries. This is a fuel structure identical to that found in debris retrieved from the lower plenum in 1985 and that was postulated to be capable of flowing, in a viscous fashion, at temperatures as low as 1350 C.5 Also found were non-porous parti-cles of Ag, Fe, and Al; Ag. Zr, U. Fe, and Ni; Fe, Zr, Ag Cd, and Ni: and Cr, Fe, Al, and Ni in a U-Zr phase. Many, if not most. Of the fuel particles 10 _B

appeared to have the darker grain boundary phase typical of the low-melting oxides of Fe. Cr. and A1. There was a very thin. 0.6-1 p complex deposition layer on the outer nozzle surface at the 283-mm elevation (top). There appeared to be no inter-action with the Inconel 600 as the composition of the Inconel was unchanged 50 from the surface. This inhomogeneous layer contained areas rich in Fe and Al. with Ag-Cd-In particles also present. The top-most part of the layer occasionally contained very small U-Zr fuel shards. The as-cut transverse sections at the 250-mm elevation exhibited some extraneous material attached to the instrument conduit and a thin deposit on l the nozzle ID: neither material was obviously similar to the fuel at 283 mm, and no further examination was made of this material. The as-cut transverse sections at the 120-mm and 145-mm elevations indicated some form of material between the instrument string and the inside surface of the nozzle, but the material had the same texture as the epoxy potting outside of the nozzle and no metallography was performed on these areas. i There were no obvious fuel masses at the 77-mm elevation (Fig. 17), but a piece of metallic Al with Ti as a second phase was between the instrument string and the inside surf ace of the nozzle. This piece was coated with fuel particles. The inner nozzle surface was covered with a 15-p layer of non-Zr-bearing 002 fuel particles. The Zr instrument leads at this elevation may be indicative of the temperature reached here. Figure 18 shows one of the leads. The microstructure is that of transformed p phase with, apparently, a trans-formation to a phase occurring at the surface. Other leads were also in vary-ing stages of transformation. Assuming the material was initially a phase, the transformation to would have occurred at 862*C if there was little oxy-gen present; the transformation temperature rises rapidly with increasing oxy-gen in the e phase. The transformation back to a on the surface, the white areas in Fig. 18. either could have occurred rapidly (minutes) if oxygen was present. or more slowly (hours) if oxygen was low. A low-oxygen level appar-ently existed because the Zr did not oxidi2e. Because there was no redox re-action with the Al 0. the temperature was <1200*C. 23 11

Another qualitative indicator of temperature at this elevation is the microstructure of the Inconel 600 nozzle, shown in Fig.19. The structure ex-hibits large grains. 0.1-0.3 mm. in dynamic movement. Annealing twins are present. The black spots are probably a tin impurity, as seen by Korth,3 and are the likely source of Ti that was found in many surface interactions on these nozzles. Unfortunately, without knowing the as-fabricated metallurgical state of the nozzle, it is not possible to make even a semi-quantitative esti-mate of the temperature reached. The fact that neither the nozzle nor the guide tube that overlapped it 6 is indicative that the material in the nozzle probably came down were damaged the guide tube and not from a flow of fuel across the lower head. Microhardness measurements were made on the transverse top and bottom nozzle sections. The hardness was 167 7 DPH at the top and 169 13 DPH at the bottom. This relative axial uniformity over -200 mm is attributed to the apparent presence of fuel essentially along the inside length of tne nozzle. C. Nozzle H5 The H5 nozzle segment (nee D10) was 146 mm long, and the segment was cut off flush with the vessel, leaving no residual stub. An elevation view of t'a l nozzle segment is shown in Fig. 20. Close inspection of the uneven lower right side of the nozzle suggests that this is part of the nozzle / vessel weld-ment. (This was subsequently confirmed by metallography of this area.) The nozzle appears to have been melted off, with candling occurring down one side. At least some of the candled material (the lowest exterior nodule was analyzed by SEM-EDX) is Type 304 stainless steel, possibly from the conduit that sur-rounds the instrument string, but diso possibly core debris from elsewhere. The top and bottom views of the as-received segment are shown in Fig. 21. The top view shows obliteration of the instrument string and filling of the nozzle cross section with molten material. The bottom view indicates a material in the annulus, but the nature of the white, smeared-appearing material filling the annulus and covering the instrument string was not established. After 12 _B

polishing, the only significant mass of material in'the annulus at this eleva-tion was a once-molten Inconel mass, shown in Fig. 22. The sectioning diagram for H5 is shown in Fig. 23. Figure 24 shows the as-cut transverse surface just below the molten top of the nozzle segment at the 114-mm elevation. Figure 25 shows the as-cut longitudinal surface through the top of the segment This section shows filling of the nozzle with both metallic (shiny) and ceramic material (shades of gray). Just below the top (Fig. 24). however, the predominant material filling the center is metallic. Figure 26 shows the mix of metallic and ceramic materials at the top of the segment. The metal is essentially Cr-depleted Inconel 600. The ceramic, typ-ical of similar analyzed areas across the top of this nozzle, is a Cr-rich oxide that contains U and Zr, probably as oxides, intimately mixed as U-rich and Zr-rich areas in what was apparently a molten ceramic (see Fig. 27); the melting point of Cr2 3 i s 1990*C. In Fig. 27. note the porosity in the Cr-rich l 0 (darkest) phase. This is an indicator of the volatility of Cr oxides, as will be discussed later. The compositions of some debris areas can be found in l Table 2. It is this " fuel" material that apparently gave rise to the fission-product peak in this region of the gamma scan. There were also local concen-trations of Al and Ti in this ceramic material. The source of the Al would be the Al 03 insulating material in the instrument leads. The Ti apparently was 2 an impurity in the Inconel 600 and came out with the Cr, both being strong oxide formers. A Cr-rich phase also precipitated as plates witnin the Cr-depleted Inconel areas, as shown in Fig. 28. This molten metal, from the right side in Fig. 25, was also found to contain dissolved fuel constituents (~9 wt.% U. -3 wt.% Zr). Areas of Ag, Cd and In were found in the surface oxide on some of the former Inconel 600 masses shown in Fig. 26. Deposits of Ag-Cd and Si, Mn, Ti, and Zr were also found within the spherical bubbles in the once-molten Inconel, similar to those in Fig. 28. A metallographic specimen was made at the 25-mm elevation to examine any surface deposits, examine the Inconel microstructure, and to perform hardness measurements. There was a 50 p-thick oxide on the surface, topped with fine 13 l

particles of debris. Although neither the particulate nor the layer were analyzed, the backscatter electron (BSE) image of the particles indicated them to be a mixture of high-and low-atomic number materials, apparently fuel and other core debris. The oxide layer had the physical appearance of Fe-oxide layers analyzed on Nozzles D10 and Ell. Nodules of Pb were found -650 p beneath the surface of the nozzle. The source of the Pb is unknown, but its morphology in the Inconel (centered in a dimple) indicates that it is not an artifact. The etched nozzle microstructure was similar to that from Nozzle L6 (Fig. 19) in that the grain boundaries were not at equilibrium and annealing twins were present. However, the grain size was larger with grains up to 0.5 mm in diameter. The bottom surface (0-mm elevation) of the H5 segment is shown at higher magnification in Fig. 29. The Type 304 stainless steel conduit is not oxi-dized. It should be noted the Inconel 600 sheathing on six of the leads is cracked in a brittle mode. The metal shards between the leads, shown in Fig. 30. are Inconel 600 plus Mn (-6 wt.%) and they are apparently the result of brittle failure of this sheathing somewhere above. The Mn source is not obvious, but it was also present in the sheathing only next to a fracture. Also shown in Fig. 30 are fuel particles and particles of Ag-Cd that also collected between the leads. The Zr leads, shown in Fig. 29, were in various .l stages of phase transformation, from - to a-phase Zr, similar to what was found in Nozzle L6 (see Fig. 18). l Metallography of a section from the bottom surface. Fig. 31, showed a dendritic structure that is typical of a weldment. This would be expected as this nozzle was cut off flush with the vessel wall, through the weld. Microhardness measurements were made on specimens from the three eleva-tions: 135 mm, 25 mm, and 0 mm. The average of measurements at the top (135 mm) was 105 2 DPH in a region that was Cr-depleted. The bottom sur-face, however, which was the weldment, measured an average of 217 13 DPH. The values from the bottom were the highest measured on any nozzle. The hard-ness at the 25-mm elevation in nozzle material was 198 8 DPh. 14

D. Nozzle HB The H8 nozzle segment was 70 mm long and a 51-mm stub remained on the 4 vessel. It was reported by MPR that -50 mm of the top of what remained of this nozzle after the accident was broken off during defueling of the lower head. Inspection of the photos of the as-received condition of the segment. Fig. 32, indeed, shows evidence (fractured leads and bent conduit) that the instrument string was broken off, not melted, even though the nozzle around it obviously had been ablated and severely necked down. It is likely that only the instrument string was holding the two segments of the nozzle together. If that was the case, the full remaining segment of this nozzle was hour-glassed shaped, similar to K11. The 137C5 gamma scan for the segment is shown in Fig. 33. The activity profile indicates that fuel is contained throughout. A likely fuel mass within the nozzle can be seen at the bottom face in Fig. 31. The sectioning diagram for the nozzle is shown in Fig. 33. The as-cut longitudinal section, shown in Fig. 34, shows that the instrument string, in-cluding its stainless steel conduit, is fairly well intact, but bent. Solidified fuel and metallic debris can be seen to the left of the string. The " goose-neck" bend of the ablated upper left corner may have occurred when the upper mating segment was broken off during the defueling operation. Analyses of the surfaces at the top of this segment identified Zr, with very little U, as the principal reactant with the nozzle. Uranium, in combination with Zr, was found in grain boundaries in the reaction areas, but Zr without U was layered on the reacted surfaces. Cadmium was also present intergranularly with the U and Zr, whereas In was found on the surface with Zr. Unlike the fuel in the tops of Nozzles M9 and H5, some of the fuel areas in the one sam-ple examined at the top of H8 were more agglomerated particulates rather than a heterogeneous solidified mass. The as-cut transverse section at the 64-mm elevation is shown in Fig. 35. At this elevation, there was a comDination of some ceramic and pre-dominantly metallic debris in the nozzle annulus. The metallic debris, shown in greater detail in Fig. 36, was essentially solidified Inconel 600 with -20 wt.% Zr and 1 wt.% U that apparently had come down in several rivulets. 15 h

Trapped in this debris were solidified inclusions of Ag-Cd. The surfaces of some rivulets were eutectic structures (Fig. 37) that contain Zr, U, and In, in addition to Ni, Cr. and Fe. Similar microstructures of primary solidifica-tion grains and eutectic structures wers found in the material higher in the annulus between the nozzle and the conduit. The quantity of Ag-In-Cd material in this debris is significant in that it indicates an appreciable amount of control materials in the vicinity of the nozzle breach, either at the 120-mm elevation or higher up at the -170-mm elevation, where the top of the nozzle had apparently melted away. It is also significant that there appears to be no obvious Cr depletion from the Inconel with subsequent oxidation, as was found at the top of Nozzle M9. It can also be seen in Fig. 36 that the outer Inconel tube of the instrument string had been under sufficient external pres-sure to collapse onto the instrument leads. The Type 304 instrument conduit was barely oxidized at this elevation. Slightly higher up, the conduit was oxidized on its inside, whereas its outside was '* protected" by molten material that had run down into the annulus. But at the very top it was entirely oxi-dized. To summarize, there were three types of fuel-bearing " debris" found in the H8 Nozzle. Unique to this nozzle was Zr and U in solidified metallic structures of essentially Inconel. In these, the Zr:0 atomic ratios were -35:1. Second, there was aggicmerated particulate (<50 p), in which the Zr:0 atomic ratios were -1.2:1. Last, there were what appeared to be solidified. porous masses; unfortunately, these were not captured in the samples analyzed by SEM-EDX. Such masses are evident in the as-cut surface shown in Figs. 32 and 34 The nozzle outer surface at this 64-mm elevation. Fig. 38, was ablated and redcted with liquid Zr that also contained a large quantity of Ni and smaller quantities of U. Fe, and Cr (Zr:U -8.5:1). The SEM secondary electron image of this area Fig. 39, shows that a Zr-rich liquid phase has penetrated the grain boundaries of the Inconel 600. Also shown in the figure are second phases that contain higher concentrations of Zr, Fe. and Cr than the matrix phase. The significance of the nature of this surface material is twofold, First, it contains all of the elements of a control rod assembly: Ag-In-Cd; 16 I

Zr from the Zircaloy guide tubes: and Fe-Ni-Cr from the stainless steel cladding. Second, the Zr:0 atomic ratio of the surface and sub-surface reac-tant. -8,5:1, is significantly different from that of the particulate fuel 1 found in this nozzle and in the fuel debris in most other nozzles where the content of U is generally greater than that of Zr (see Table 2), These two points strongly suggest that this nozzle was in contact with material from the control rod assemblies before the major fuel flow arrived on the vessel. Microhardness measurements on the nozzle averaged 133 4 DPH at the 64-mm elevation and 148 7 DPH at 108 mm. These values were among the lowest values measured on inconel that did not exhibit Cr-depletion and reflect a-high nozzle temperature 64 mm from the vessel. E. Nozzle D1H The D10 nozzle segment (nee H5) was 235 mm long, leaving an mm-long stub on the vessel. An elevation view of the nozzle segment is shown in Fig. 40. Close inspection of the beveled top of the nozzle indicates that d -13 mm of the top had melted off. There were a number of noteworthy features on this nozzle. The top 75 mm appear to have a crust with wide, shallow depressions. The middle 75 mm are covered with a crust that is thicker and quite porous, and only on one side of the nozzle, indicating its deposition was unidirectional. The 137Cs activity profile (Fig. 42) indicates that there is a small amount of fuel at the very top of the nozzle and that the porous debris contains fuel as well. (Subsequent sectioning through the debris, described below, ' indicates that there was more fuel mass attached to one side of the nozzle than inside the nozzle at the elevation of the section. The gamma activity, therefore, was principally from surface debris.) Just above tne midplane bevel is a crack. -20 mm long, that penetrates the nozzle body. The surface debris and scale terminate just above the cut-off elevation -75 mm from the bottom of the nozzle. The top and bottom views of the nozzle segment are shown in Fig. 41. The top view shows that the in-strument string has been generally melted, with melted material probably the 17 f

missing top 13 mm, filling the nozzle's annulus. Candling down one side can be seen. The bottom view shows the instrument conduit to be intact with what might be fuel fragments on one side of the nozzie's annulus. The sectioning diagram for the D10 nozzle is shown in Fig. 42 together with the gamma activity profile. The segment was cut into nine major pieces, from which 13 smaller specimens were generated for detailed examination. The longitudinal section through the top of the nozzle. Fig. 43, shows melting of the instrument string, severe damage to the stainless steel conduit. and the melted Cr-depleted Inconel that filled the annulus around the conduit. The ceramic-appearing material on the other side appears to be, based on the M9 analytical results, a fuel-bearing oxide of Cr. (The sample from this ceramic region was lost during metallographic preparation.) Only fuel in the form of shards was found in a metallographic section from the instrument-tube side of this section (Fig. 44). The compositions of such particulute areas are given in Table 2. The significance here is the particulate and inhomogeneous nature of the debris within the melted metallic structure of this nozzle, unlike the tops of M9 and H5. The surface of the nozzle at the top was ablated with evi-dence of U-Zr imbedded in the Cr/Ti-rich surface. Aluminum had advanced -200 p into the nozzle beyond the Cr/Ti oxidation areas, and was usually as-sociated with Mg the source of which is unknown. Cadmium was sporadically located on the surface. Silver and Cd nodules that also contained U-Zr were located in seemingly unaffected Inconel at least 300 from the surface. The transverse section at the 266-mm elevation. Fig. 45 showed exten-sive damage to the instrument string and conduit and possibly some fuel debris 1 in the annulus but none on the exterior. The exterior surface at this eleva-tion exhibitej an alternating pattern of interacted / ablated areas and areas showing little evidence of attack. The interacted areas, which would be the shallow depressions shown in Fig. 40. were up to 2 mm deep and consisted of both sub-surface-affected zones and layered deposits of debris and reaction pro? c.ts on the surface, as shown in Fig. 46. Aluminum was aggressive in in-teracting beneath the Inconel surface. On the ablated surface. Cr and Ti. likely as oxides, formed a thick layer, with an additional Cr-rich layer con-taining control assembly fragments on top of it. The outermost layer was 18 _M

I almost pure Fe (oxide). In some areas this layer contained fragments of a mixture of U-Zr and Ag-Cd. On surf ace areas where there was no ablation, the surface layer was -1 thick and contained Al, Zr, Ag, Cd, In, Ti, Cr, Fe, and Ni, but no fuel. The transverse section at the 177-mm elevation, Fig. 47, shows an area of fuel debris on the exterior surf ace, solidified metal in the annulus, oxi-dation of the conduit, collapse of the central Inconel 600 tube, and large bubble formation in the Inconel on the surface of the nozzle. Almost all of the surface damage was limited to one side, an arc of -180". At the 158-mm elevation, Fig. 48, the surfacc damage extended farther around the nozzle. A solidified ingot of what proved to be Inconel was inside the annulus. This ingot contained imbedded particles of solidified Ag-Cd, generally at a ratio of 10:1, as did the adjacent nozzle body. There was no evidence of foreign elements on the apparently ablated surface, only layers rich in Cr, Ti, or Ni. There was an extensive area of intergranular separa-tion on one side of the nozzle body, adjacent to the surface crack that was visible in Fig. 40. This area, shown in more detail in Fig. 49, was exten-sively penetrated by Ag-Cd. both as stringers, Fig. 50(a), and discrete parti-cles Fig. 50(b). Many of the larger cavities appear to be grain-boundary separations, or grain boundaries that have been dissolved by a penetrating liquid, such as Ag-Cd. In some cases, the protuberances on the surfaces of the cavity were sufficiently rounded to have the appearance of having been molten. Some of the larger cavities were filled with shards of fuel in a ma-trix of Cr-oxide, as shown in Fig. 51. The compositions of some of these shards are given in Table 2. Aluminum. Cr, and Fe, all Strong oxide formers, were found in the grain boundaries of one such fuel particle. The etched mi-crostructure of this area. Fig. 52, indicates a very large grain structure with a possible second phase in the grain boundaries. The nature of this grain-boundary phase was not actually determined; only Ag-Cd. as in Fig. 50(a), was determined in the SEM-EDX analyses. The average microhardness of this area was only 124 2 DPH, indicating that a very-high temperature was achieved. The area was not depleted in Cr, however, as was the case in other low-hardness areas. 19

[ Although. a cast, dendritic microstructure was' not brought out metallo- ] graphically, it is not inconceivable that at least one~ side of the' upper part. of this nozzle was essentially molten, or very close to it, the apparently t undisturbed exterior shape notwithstanding. Measurements on the nozzle cross section in Fig. 48 indicate that not only is the center hole eccentric but the f outer surface is as well. The outer surface has moved outward by -3.5 mm op-f posite the eccentricity of the ID. The fact that the inner instrument tube is i r collapsed at this elevation is evidence that there was a high internal pres-sure in the nozzle that would have been the driving force to move the weak l r side of the nozzle outward. The large surf ace bubble at 177 mm is another in-dication of melting of at least the surface. Assuming the fuel flow enveloped { the nozzle from the bottom up, a fuel crust could have rapidly solidified against the nozzle forming a mold in which areas of the nozzle rapidly melted, at -1400*C, and then solidified, trapping some fuel debris and control rod ma- [ terial inside. The rough nature of the surface of this nozzle can be con-l trasted to the smooth surface of the ablated areas on the surface of Nozzle l H8. I r s The massive surface deposit diametrally opposite to the intergranular [ l separations is shown in Fig. 53. It is assumed that this type of deposit is -{ typical of the thick deposit on this side of the nozzle between the 120- and 180-mm elevations. This complex structure is a combination of solidified i Cr-depleted Inconel (white areas) and physical mixtures of oxides of Cr. Zr. j U. Fe and Ni (gray areas). Part of the original nozzle surface is assumed to j be the thin gray line of Cr and Ti (oxide) at 5 o' clock in the figure and ex- { tending upward through the wide cand of voids to 12 o' clock. The gray phases { to the right of this line are principally Cr. A1. and Ti rich, with some U and { Zr. The Inconel matrix to the right of these oxides contains inclusions of f Ag-Cd. as does the large Cr-depleted Inconel masses between 6 and 8 o' clock. 1 These inclusions are shown in Fig. 54. Their nominal compositions were in the range of 70-80 wt.% Ag 30 wt.% Cd. A fuel-containing area is a triangu-l lar-shaped particle at the outer edge of the deposit shown in Fig. 53. The i microstructure of this area. Fig. 55, shows segregation of the fuel into a U-i rich phase (89 wt.% U-3 wt.% Zr-8 wt.% Fe) and a Zr-rich phase (25 wt.% U-57 t wt.% Zr-18 wt.t Fe). Such fuel concentrations were the exception. Generally. 20 [

.-.. ~ - - ~- 7 i i -l fuel constituents were more randomly dispersed in other phases of Cr'and Fe i oxides. The areas containing the larger amounts of U and.Zr were in the outer. -areas of the deposit. i Figure 56 shows the instrument string at the'158-mm elevation. The Type j 304 stainless steel conduit was almost completely oxidized but the.Inconel 600 f inner and outer instrument tubes were not; there was only a small amount of oxidation on the outer tube. The inner tube had collapsed from external pres-sure and was filled with solidified Inconel, slightly deficient in Cr. The Zr .[ t instrument wires had reacted to varying degrees with Al 023 insulation, result-ing in oxidation of the Zr and reduction of the Al 03 The relative free ener-l 2 gies of formation of these oxides suggest that a temperature of at least i i 1200*C was reached for this redox reaction to occur. One instrument wire, at j j 5 o' clock in Fig. 56 and shown enlarged in Fig. 57, apparently had melted and { i j sent six stringers outward toward the cladding. An analysis of one such j stringer indicated only Zr, but, because the melting point of Zr is high at l l 1850*C, it is more likely that the stringers are the eutectic of Al and Zr at a melting point of 1350*C. This is more in keeping with the -1200*C minimum ~ temperature for the redox reaction. One stringer reached the sheath and 3 caused local melting in the wall. Although the melting point of Inconel is -1400*C, the localized melting could have occurred at a lower temperature be-l cause the Zr-Ni eutectic occurs at 960*C. In any event, the temperature of s the instrument string at this elevation was at least 1200*C. l }' There was a 0.25-mm-thick layer of debris on the surface of this nozzle at the 82-mm elevation. The debris. a section of which is shown in Fig. 58, was multilayered immediately adjacent to the nozzle. The innermost reaction zone was somewhat depleted in Cr and Fe and contained 9.5 wt.% In. Moving outward. the zones contained an increasing amount of In. combined principally l I with Ni. with up to 95 wt.% in (balance Fe) in the outermost of the inner re-l An intermetallic. Ni In7, was one such zone. The blocky gray l action zones. 3 mass that was the principal constituent of the 0.25-mm-thick layer was Fe { (oxide). Small particles near the reaction zones contained Cd and In. Large ] fuel shards of various compositions were trapped in the Fe (oxide) matrix. i ) 21 -l l

~ t The compositions of these various particles, or specific phases within these l particles.(denoted by a number), are summarized in Table 2. l

t Microhardness measurements made on the nozzle body at the 82-mm eleva-i tion gave an average hardness of 161 4 DPH for four values.

i t i The surface layer at the 69-mm elevation was only 1-10 p thick. In the thinnest areas of the layer, random particles of fuel (82 wt.% U-12 wt.% Zr) { were imbedded in the surface. As the surf ace layer became thicker, the undere lying reaction zones into the nozzle surface, -5 p wide, contained Al, Si, Ag, Cd, In, and Sn in addition to Ni, Zr, and Fe. The thickest outer layers con-sisted of partial bands containing U, Zr, Ag, Cd, In, Sn, Mo, and Al in addi-l s tion to Fe, Ni, and Cr, in various combinations. Where Zr and U were found } I together, the Zr:0 atomic ratio was very high, i.e., >10:1. The microhardness of the nozzle at the 69-mm elevation was an average 168 10 DPH, essentially the same as it was 13 mm above. j F. Nozzle Ell j The Ell nozzle segment (nee L6), shown in Fig. 59, was 225 mm long. The [ base of the nozzle was 221 mm above the lowest point of the vessel. After severance from the vessel, an ~77-mm stub of the nozzle remained with the 'ves- -[ 1 sel. The nozzle surface was bright and apparently unaffected by the accident over about half of its length. There was a loosely adherent scale over the t upper 145 mm and part of tne bottom 38 mm. The tapered top of the. nozzle was I i wrinkled and -3 mm of the top was missing, but as will be seen, this material l melted and ran down into the nozzle. Figure 60 shows the top and bottom views l of the nozzle segment. The top view indicates that nozzle material had en-I tered the annulus between the instrument string and the nozzle ID, and the t-string is visible in the top view. The bottom view shows the string partially withdrawn and it subsequently fell out on handling. From subsequent section-ing, it was apparent that the string had separated -25 mm from the top of the i nozzle. The cause of the separation was not determined. The 137Cs activity I t profile for the segment, Fig. 61, indicates that there was fuel in the top f ~15 mm of the segment and in an area between the 210- and 250-mm elevations. j I 22 i

The segment was sectioned transversely and the upper end was sectioned longitudinally to investigate. principally, the possible fueled area indicated in the gamma scan. The basic sectioning diagram is shown in Fig. 61. Figure 62 shows the transverse section through the 274 mm elevation and the longitudinal section through the top piece just above it. The instrument con-duit is visible in the longitudinal section but not in the transverse section, indicating that the instrument string had been severed at this elevation. An enlarged view of the material in the top of the nozzle is shown in { Fig. 63. The principal components of this debris were fine (<100 p) particles of fuel and nozzle debris that formed a matrix in which large fuel shards and f oxidized pieces of the conduit were trapped. Some fuel particles in this re-gion showed segregation into U-rich and Zr-rich phases, which is indicative of relatively slow cooling from the solidus temperature. The large shards, how-ever, showed no such segregation and appeared to have solidified very rapidly. i There were Ag-Cd particles trapped in some of these fuel areas. The composi-tions of some fuel areas and particles are given in Table 2. The principal non-fuel constituent in this matrix of debris material was Fe, not Cr as in l other nozzles, j l The inner and outer nozzle surfaces at the top were severely attacked by Al, presumably from the Al 023 insulation in the instrument string. Titanium and Cr were also strongly evident in surface interactions, it is assumed that the Ti was an impurity in this Inconel 600 and came to the surface, as did Cr, e under the strongly oxidizing environment. The outer surface apparently was sufficiently hot and plastic to form " micro-folds" that trapped particulate l matter (see Fig. 64). The particulate consisted of fuel (see Table 2 for com-position) and Zr, Cd-containing particles, among others. The ablated surface was covered with an apparent oxide layer of principally Cr and Ti. { -l Examination of the transverse section at the 274-mm elevation showed a that the solidified metallic material on the inside surface was contiguous i 1 with the nozzle with a composition essentially that of Inconel. Areas of the i i 1 surface of this material had undergone post-movement reaction with A1. The ceramic material attached to the inner surface was a loose agglomeration of 23 f

particulate shards- (Fig. 65) that included fuel, fine fuel particles -in an Fe-j oxide matrix, calcium-silicate, Fe-Ni alloy, and an Ag-Cd/ fuel-Fe agglomerate. 1 Apparently insufficient fuel / fission products were present'in this material to t cause an indication in the gamma activity profile at this elevation, The outer surface at this elevation contained areas of-surface scale, j about 10-20 p thick, and other areas of surface attack. The outermost par'c of the scale contained Ag (11-45 wt.%) and Cd (4-15 wt.%), the balance being f Al, Fe, Si, Ni, and Cr in descending order of content. The inner part of the scale consisted more of the latter constituents. A reaction area, shown in. i Fig. 66, contained Ag, Cd, In, and Zr in addition to Fe, Ni, Cr, Al,-and Si. j Silver-cadmium nodules were found up to at least 1 mm into -the nozzle. i e i Hardness measurements taken near the inner and outer surfaces all indi-I cated a hardness in the range of 136-141 DPH (average of 137 4 DPH). This is significantly lower than the hardness closer to the nozzle top only 15 mm f above. l I The transverse section made at the 220-mm elevation to intercept the { gamma peak there is shown in Fig 67. Except for a small, ceramic-appearing mass on one side of the inner surface, there was no obvious cause of the gamma i peak and no metallographic section was made at this location. It can be as-i sumed that the ceramic-appearing mass is similar to the material found at the [ 274-mm elevation. i The outer surface at the mm elevation exhibited a flaking, 0.13-mm- { thick scale (Fig. 68). The scale consisted essentially of fuel particles in a matrix of Fe-oxide, similar to the scales found on the outside of the other nozzles. More significantly, however, immediately on the nozzle surface be-neath the thick scale was a 10-p scale that contained imbedded particles of Ag-Cd, as shown in Fig. 69. This thin scale is strong evidence that a Ag-Cd-containing debris layer existed on the vessel before the massive fuel flow oc-l t curred. The hardness of the nozzle at this elevation was -190 DPH. about that 24 4

L o i .of unaffected Inconel 600, indicating that the nozzle did not get exception-ally hot at this elevation. i 1 VI. DISCUSSION j .I A. Definina " Debris" .I It is appropriate at this point to define " debris" as it will be used in i this discussion. Fuel '* debris" is defined h'ere as the material that flowed to f the lower head 226 minutes into the accident. Temporally and positionally ] this debris could have been liquid, liquid plus solid (" wet sand"), or solid (a crust against the vessel, nozzles, guide tubes. or anywhere on the surface of the solid / liquid material that is below the solidus temperature for that { heterogeneous mass of material). From these examinations or others that have l been performed, it is not possible to distinguish between the debris as de-fined here from other fuel that may have arrived on the lower head earlier than the 226-minute demarcation. Therefore, all fuel debris, with exceptions l to be noted, is cons) Nred to be from the same source, whether the material is " companion material," from the " lower debris bed," or on the surface of noz- { zles as a thick crust or a thin scale. A debris " bed," or crust, of this ma-terial would only be that portion of the " fuel debris" that had solidified. i.e., no liquid phase, either upon initial contact with the vessel. or subse- ] quently after all of the liquid had solidified wherever it came to rest. I Thus. "the" debris bed, or crust, on the lower head would have 'a changing ' character with respect to time and location as the fuel solidified, depending upon local temperatures and geometry of the lower head. This distinction is { made in this report when discussing the damage to individual nozzles, j In addition to " fuel debris." this report will discuss " control rod as-f i sembly debris," consisting of all the major constituents of a control rod as-l sembly: Ag, In. Cd, Zr, Sn. Fe, Ni. and Cr. Fuel rod materials would be mi-- i nor constituents in this debris, and it is difficult to distinguish whether their involvement was early in the accident or later af ter the " fuel debris" l f reached the lower head. It will be shown later in this discussion that there 1 25 i

j 4 i is substantial evidence to conclude that there was a bed of " control' assembly debris" on the lower head before the fuel debris arrived. B. Nature of Nozzle Damace l The six nozzle segments examined at ANL fall into essentially two cate-gories: (1) nozzles destructively affected by molten fuel: H8, H5. and M9: i and (2) nozzles thermally affected by fuel debris but outwardly exhibiting i little damage: L6 and Ell. Nozile DIO f alls into a-middle category that, de-pending upon interpretation, encompasses both categories. l I The tops of Nozzles H5 and M9 were destroyed directly by molten fuel. i The intimate mixing of molten fuel-bearing particles with molten nozzle and instrument string materials is evidence for this conclusion. Because only the { lower part of the remaining H8 nozzle was received at ANL, it is not possible to say positively what the mechanism for severance was at the -170-mm eleva-i tion. However, with a total remaining height of only 170 mm. it may be as-l sumed that the nozzle was melted off in a manner similar to that which oc-curred with Nozzles M9 and H5. and apparently G5. The finding of what appears s s to be porous fuel in the bottom of the H5 segment supports this conclusion. Although Nozzles 010 and Ell did not melt-off as dramatically as M9, H5. and ~! H8 their tops did melt, as evidenced by the metallic debris within the noz-zles. f Nozzles L6, H5, D10. and Ell were found to be covered, to varying de-grees with an Fe-(oxide) surface scale that ranged in thickness from a few microns (L6) to 0.25 no (D10). The thick crust patches on one side of D10 are similar in nature, i.e., Fe-based, but these patches also contain an abundance of molten inconel and Cr-oxide, which makes them different in nature but not 't in source. What is probably a similar scale near the top of M9 just beneath I the melted portion was not examined. These Fe-based scales are different from [ the porous Cr-based ceramic that was prevalent in the top of the nozzles that j melted. M9 and HS (and probably H8). The Fe-based scales are barely adherent l to the nozzles and do not appear to have grown from the base metal.7 Because of its apparently non-nozzle nature, it is believed that the source of the Fe-l l 'I f 26 i i

-= _= 1 1 l. l i based exterior scales and the Fe-based matrix in the top of Ell was-the fuel j c l flow that melted its way through stainless steel structure on the way to the l lower head, regardless o' its exact path. These Fe-based materials are gener-ally located in temperature regimes that are between that of molten Inconel and that of the very clean nozzle surf aces at the cooler lower elevations. It I is not obvious why these Fe-based scales contain only adventitious pieces of I core debris and not material more akin to the ** companion" samples.1 Chromium l 1 a l apparently is not present in these scales because Cr-oxides are very volatile { I above 1000*C and would have migrated out of the debris during the movement to l l t the lower head. In contrast. the Cr-oxide that formed at the tops of the { nozzles when they were melted by molten fuel stayed in place, indicating very rapid cooling. (Rapid cooling of the molten nozzle tops is also evidenced by a general lack of rundown of fuel-bearing debris in most nozzles, with the .f noted exception of the exceptionally hot HB). The bubbles formed in the re-mains of Cr-depleted Inconel were likely caused by Cr-oxide vapor, which ap-f parently precipitated into the platelets found in the H5 microstructure when the vapor could not vent to a free surface. The assumed hour-glass shape of the "whole" remaining H8 nozzle, of which ANL received only the bottom part, may possibly be explained by the finding of extensive surface interaction between a Zr-rich phase and the noz-f zie. There is sufficient evidence (see next section) to conclude that there [ was a debris bed of control assembly materials on the lower head before the l f major fuel flow occurred at 226 minutes. The depth and nature of that bed cannot be determined because any direct evidence of it was obliterated by sub-sequent fuel flow. However, it is clear that liquid Zr, from this bed, was a primary ablating agent on the surf ace of the H8 nozzle and that the source of that Zr, without significant quantities of U but with Ag-Cd, was control as-sembly components. The appearance of the D10 nozzle surface (rough, craggy, and crusty) may be contrasted to the comparatively smoother surf ace of the { necked-down region of H8. Nozzle D10 was in contact principally with hot fuel I at temperatures sufficient to possibly have caused melting on one side. Nozzle H8, on the other hand, was in contact with Zr, which has a eutectic with Ni at 961*C. This lower temperature for liquefaction of H8 likely caused [ the severe necking down and smoothing of the surface compared to D10. An es- { 27

4 l timate of the minimum depth of the Zr-containing debris on the surface before j the fuel flow re-melted it would be -120 mm. the height of the bottom portion of the nozzle segment. A maximum height might be an additional 50 mm, if the j i. ablation was truly hour-glass shaped. l C. Eastulated Fuel Relocation Scenario a The differentiation of Fe-matrix debris from Cr-matrix debris makes pos-l sible postulation of a fuel movement scenario and estimations of initial f " debris bed" depths at the nozzle locations: the final " debris bed" depths would be those measured by MPR Associates during the defueling operations. The postulated fuel movement scenario and estimation of the initial debris-bed l depths are described below. f I i The external scales combined with known nozzle melting provide a quali - } tative assessment of the axial temperature profiles of the nozzles. The scales were adherent in obviously hot areas (e.g., beneath the melt zones of M9 and H5) and less adherent in the lower, colder region near the vessel. The j finding of even thin scales near the bottom of some of the nozzles (not all i nozzles were extensively examined for scale formation at every elevation) in-j 1 dicates that all the nozzles were likely surrounded by a debris bed that was l i l colder against the vessel and botter above. This is consistent with a fuel !t flow that moved down and across the lower head in a lava-like movement, gener-ating a solid crust against the vessel and the cold nozzles it contacted. { i This crust apparently cooled sufficiently fast to result in no surface inter-action with the lower portions of. perhaps. the first nozzles.it contacted. In effect. this cold crust protected the lower portions of the nozzles from the hotter fuel debris above. Above this crust would have been a liquid-solid [ l mixture (~ wet sand") of high-solidus-temperature material (U-2r oxide phases) i and lower melting materials (Al, Fe. Cr oxide eutectics). Above the " wet i 1 i l sand" would have been the liquid ** core" of the flow, and above that some sort [ of thin crust that formed in contact with steam. In such a lava-like flow. I e the initial basal crust would have been thick because the cold vessel. acted as { [ an excellent heat sink. As the flow moved, the vessel would have heated up and the ensuing crust would have been thinner. At some point in the movement, 2b I

m -. __ i 4 a apparently in the E7-8/F7-8 area, the basal crust could have become suffi-i i ciently thin to diminish its insulating properties and a hot spot in the VEs- ] sel developed. Continued movement of the flow would have brought sufficiently 1 het fuel to one side of the D10 nozzle to form the thick crust and then en-1 i l velop the entire nozzle at some temperature higher than the solidus tempera-ture of Inconel 600, As described previously, it is postulated that an effec-tively simultaneous cooling of the fuel debris and surface melting of the noz-zie resulted in entrapment of fuel particles beneath the surface of the nozzle and the cratered appearance of the surface. The bulging of the. weak side of i the nozzle would hava occurr ed at this time. The adjacent and slightly ele-j vated Ell nozzle was affected only to the extent of fairly extensive scale formation, surface melting (" pruning") of its tapered top, and melting and { i j collapse of its top 3 mm. The finding of the Fe-based debris in the top of l s 4 l the nozzle indicates that some of the fuel flow came straight down as it j j passed over the nozzle, but it was too cold to cause more than superficial l 1 1, surface melting of the nozzle tip. i e f 1 (It must be pointed out that there is no direct evidence for such a j j lava-like flow moving in contact with the vessel, An alternative scenario j would have the same layered lava-like flow, but elevated, by perhaps a steam vapor, as it moved through the water in the lower head. As it lost momentum, it could have dropped to the lower head at E7-8/F7-8, causing the vessel hot spot. The explanation of the elevated melt-offs of Nozzles M9 H5 and H8 would be the same, as would the effects on the other nozzles.) In the lava-like surface movement scenario, a " debris bed depth" can be estimated for five of the six nozzles. If one applies the definition that the debris bed is the solid crust that is formed beneath the liquid fuel, then the elevation of melting on a given nozzle, i.e., the elevation at which liquid fuel melted the nozzle and interacted with it, would be the effective thick-ness of the debris bed at the time the nozzle melted. However, what was be-lieved to be candling of metallic debris down the side of the H5 nozzle could not have occurred if there had been solid debris at a level just beneath the melted area. However, two points should be considered. First, the candled material had a composition closer to Type 304 stainless steel than to inconel 29

.. y, if i r i 600 and its source may not have been-the H5 nozzle but rather the' moving f debris itself. Second. the failure of individual nozzles may have been caused -) i by fuel coming.directly from above before debris built up along the sides. In that case, the instrument string conduit would be the likely source of the stainless steel, d An alternative fuel-flow direction is appropriate for H5. and perhaps f other nozzles, for another reason. Considering that the nearby H8 nozzle ap-parently melted off at -170 mm. the relative elevations of the nozzles (see j Column 1 in Table 1) would mean that H5 melted off -83 mm above the melt-off + of H8. This would mean that these two nozzles could not have been melted off t a by the same liquid level in a stagnant or moving pool. The same argument'can. a ] be used for the M9 nozzle, which melted off some 230 mm above where H8 appar-ently did. In the case of M9 however, it could be argued that the flow at ] that point was moving downhill and the basal crust was very thick because the vessel was still relatively cold. (Please note that the G5 nozzle segment. now at INEL is similar in height to the adjacent H5 segment and could have l been melted off by the same height of liquid as H5.) The implication here is that H5 and G5 were melted by a downward-moving pool and that they were melted l before the pool reached HB. Both the H5 and G5 guide tubes were melted off ( significantly above their respective nozzles, indicating that such a moving j pool was deep as well as elevated. Directionally, this flow would not be in-l l consistent with the location of the vessel hot spot: Nozzle G6. just beyond + H5. was apparently melted down to a small stub on the periphery of the hot l spot. 7 1 i i + Given the lava-like flow scenario and its attendant debris bed height / nozzle melt-off characteristics, the significant differences between Nozzles L6 and M9 suggest that multiple fuel flow paths existed and that the flow across the lower head was not one massive unified flow. Nozzle M9 sug-5 gests a deep basal crust and a high liquid level, consistent with a fresh fuel } i flow contacting the vessel, with a direction toward H8 and the eventual hot j spot. The cleanliness of Nozzle L6 indicates that there was no large liquid flow coming from the southeast between H5 and M9: although the bottom of the adjacent KS guide tube was damaged, the K5 nozzle apparently was not. The a 30 q +

~ i i i l l surf ace debris found on L6 woulo have been material from the periphery of the j flow, or simply adherent material when the fuel debris eventually settled to form the " companion material." j The fuel material inside Nozzle L6 is believed to have come straight i down the guide tube and not from a lava-like fuel flow for the following rea-j 1 sons. First, both the L6 nozzle and its overlapping guide tube were virtually unscathed, and it wouis have bet difficult, albeit not impossible, for a rel-- atively rigid lateral flow to have made its way up into the guide tube and t then down into the nozzle. Second, there was an unreacted fuel pellet segment j t inside the nozzle. Such a piece would not have survived in that form in a hot i fuel flow. Third, the L6 nozzle was beneath a control rod, and appreciable numbers of Ag-Cd-bearing particles were found in the annulus. Fourth, fuel j that had been melted contained Fe. but the transformation into U-rich and Zr-rich phases was incomplete, indicating relatively rapid cooling. This was not typical of transformed fuel found in the hotter nozzles. Even though the ma-j trix binding the. particulate was Fe-based, this material would have had a sim-i'.ar history to that in the lava-like flow, except its movement would have been only downward. In the overall scenario, the source of this potpourri of material is almost irrelevant. The significance of its presence is that it f i apparently generated sufficient internal heat to anneal the Inconel 600, as j evidenced by the relatively low and axiall, uniform microhardness values for i L this nozzle. l l D. Presence of Control Assembly Materials I Four of the six nozzle segments examined at ANL were'under control rod f assemblies: M9. L6. H5. and H8. One. D10. was beneath an axial pcwer shaping l rod that contained 914 mm of Ag-in-Cd clad in stainless steel. The last. HS. was beneath a burnable poison rod that contained Al 03-B4C pellets clad in 2 Zircaloy. There is pervasive evidence from the ANL examinations that the as-semblies containing Ag-In-Cd f ailed relatively early during the accident and j t j that the debris from these assemblies deposited in some form, probably as solid particulates. on the lower head befcre the principal fuel flow occurred { at 226 minutes. In this sectibn will be summarized the evidence to support l t i I 31 ,- I

= i 1 i this conclusion. This material being on the lower head when it was may be a factor in determining the margin-to-failure of the lower head. There is no direct, unequivocal evidence that the postulated control rod debris bed existed on the lower head. Examination of companion material l = found no such evicience, either because the sampling of the "hard pan" was ran-l dom and not site-specific, or because the analytical techniques were too gross j to identify what would be a small percentage of the fuel debris. Most, if not. j all, of such a control rod debris bed would have re-melted when it came in f contact with even the basal crust of the fuel flow; possibly it would have l been consumed into it. Therefore, evidence for such a bed would now be, at i 1 best, on a microscopic scale and fortuitously derived. [ The first evidence that the control materials were on the lower head be-i fore the fuel flow arrived was the finding of Ag-Cd nodules and In-Fe-Ni-Zr i f phases solidified in. situ in the vessel cladding cracks in the E6 and G8 boat l Samples. The only fuel present in the cracks was apparently adventitious shards that likely fell in during defueling. Had there not been a control rod i debris layer present when the fuel flow occurred, there would be no reasonable 1 explanation for this finding. These materials would not have segregated in r j that manner from the partially solidified fuel flow. f The overwhelmingly Zr-rich liquid that contained Ag-Cd masses and ab-f lated the H8 nozzle is further evidence for the presence of the control rod j 4 i debris bed. The Zr:0 ratio of -8.5:1 was far in excess of the Zr/U ratios [ found in fuel masses that were analyzed. This excess of Zr would be from the b Zircaloy shroud tubes in the control assemblies. The minimum depth of this .[ Zr-containing debris bed was -120 mm. ( ] q The findings of Ag and Ag-Cd inclusions deep beneath the surfaces in j 4 I most of the nozzles in a form of liquid metal penetration indicates that there r l was a layer of control materials either adhering to the surface ready to be { melted when contacted by the hot fuel, or there was a thick debris' bed up against the nozzle that would yield the same result. That liquid Ag-Cd had f i penetrated the inconel nozzles somewhat before nozzle melting occurred is evi-l t f i 32

t i denced by the apparently vapor-pressure-derived' bubbles in the Inconel that contained Ag-Cd and other core debris constituents, j i Perhaps the most striking evidence for the superposition of Ag-Cd be-4 neath fuel debris is shown in Fig. 69, where 10- particles of Ag-Cd are be-neath a fuel debris scale on Nozzle Ell. } Because the ANL nozzles were almost all beneath control rods, the pres-ence of such debris on or in the immediate vicinity of the nozzles could al-most be expected. Given the narrow 4-mm annulus between the instrument string. [ l and the inside of the guice tube, debris coming from directly above would be ( fine particulate. Indeed, such fine particulate was found on the top of L6, l 4 as well as at the bottom of Ell. However, whether this material came down di-rectly from above or was circulated to the lower plenum by the coolant pumps is not the issue. (Such a distinction might be made by examining other noz-zles that were not beneath control rods. The ANL findings for H5, which was not beneath a control or axial power shaping rod, showed some Ag-Cd in molten l masses but only minimally on exterior surfaces and none in the Inconel.) The-r material in the cracks in the boat samples and the Zr attack of Nozzle H8 is sufficient evidence to conclude that there was a stagnant control material de-bris bed of some. unfortunately, undetermined depth and breadth. t i E. Temnerature Indicators t i r A principal objective of the nozzle examinations was to provide quanti-tative data on the temperature of the nozzles in proximity to the vessel. l This objective was satisf'ed only to a limited degree. The principal reason for this was the lack of time-temperature annealing data for archival Inconel 600. Korth's work using Gleeble tests on non-archival Inconel 6003 provides l insight, but quantification using grain size and hardness data cannot be abso-lute. The following discussion is an attempt to glean some relative, if not-quantitative information, from the ANL examinations. l i j 33 i ~ 1 m 8

l 1. Hardness Measurements I The microhardness measurements on the Inconel 600 nozzles, summa- { rized in Table 3. are essentially in qualitative agreement with what was found by observation. The data from Cr-depleted areas should be disregarded because t the values do not represent Inconel 600, only a Ni-Fe alloy of. varying compo-sition. Likewise, the value for the hardness of the top of Ell, which par-l tially melted, is inexplicably high and should also be disregarded as not. rep-l i resentative. It appears that the nominal hardness of the as-fabricated mate-l rial is -200 DPH, considerably higher than the 155-160 DPH range for Korth's l material. The most significant data is from H8. where the hardness 64 mm from i the vessel was 133 DPH. a value that Korth's data indicate is achieved in 10 l 3.inutes at -1000*C. Following this line of reasoning, r,one of the other nozy f zles within 70 mm of the vessel achieved 1000*C. It is interesting to note .f that the Zr surf ace ablation of Nozzle H8 would have begun at the 961*C Zr-Ni eutectic, a temperature well in keeping with the 1000*C estimated from the hardness measurement. } l 2. Microstructure ) The microstructures at the 77-mm elevation in L6 and the 25-mm ele-vation in H5 showed active grain growth, which Korth's data indicate a temper-ature of at least 950*C was reached. Because the grain size was so large in f H5. 0.5 mm. the temperature may have been higher, or the time at elevated tem-perature longer. Grain size and growth kinetics are highly dependent upon metallurgical history. Because Korth's material was not truly archival, this correlation should be viewed with skepticism, particularly since it does not i l agree with the hardness correlation, i i 3. Penetration by Aa-Cd r i A Ag-Cd alloy with a nominal composition of 80 wt.% Ag-20 w.t% Cd. I r typical of the deposits found, melts at -860*C: Ag melts at 960*C. Liquid i penetration occurred only in the upper elevations of the nozzles where such t temperatures would be easily achieved. Lack of such penetration nearer the j vessel suggests that either the nozzles did not achieve that temperature, save f i ~.. _,

H8 or_there was insufficient Ag or Ag-Cd to penetrate. or our analytical techniques simply did not see it. 4 Miscellaneous Indicators Qualitatively, a good indicator of the axial temperature profile'in a nozzle was the presence and then the relative adherence of the fuel debris scale on the outside nozzle surfaces. For all nozzles except L6. Which has no obvious external scale and apparently was not in a flow path, there is a rea-sonable correlation between scale location and nozzle hardness. On nozzle D10. the scale was adherent at the 82-mm elevation, which had a hardness of 161 DPH. That hardness is above Korth's breakpoint at -1000*C, where Inconel apparently anneals rapidly and the hardness f alls to -130 DPH or below. With this correlation, it could be subjectively concluded, again, that only Nozzle H8 had a high temperature near the vessel. The temperature of the other noz-zies would have been less than 1000*C below the following elevations: M9 215 mm H5 38 mm 010 82 mm Ell 255 mm Deriving nozzle temperatures from the condition of the Zr instrument leads is considerably less direct than using any other indicator, because the leads were insulated in Alz03 and the radial heat transfer path to the nozzle is impossible to calculate. The observations on -to-a transformations only establish a minimum threshold of 860*C, which was likely achieved in most noz-zles. The 1200*C threshold temperature for the Zr/A103 redox reaction would 2 be a good indicator except for the heat transfer issue. It is significant. however, that the 158-mm elevation in D10, where this reaction was obvious, is also the elevation where the hardness was the lowest for that nozzle, 124 DPH. F. Penetration of Materials into Nozzles The penetration of gamma-active materials downward into the nozzles was estimated from the 137Cs gamma activity profile, and results are summarized 35 j

{ 8 I t in Table 1. It was assumed that the gamma activity was associated with fis-i sion products in fuel and, therefore, the results are reported as " fuel pene-I tration," Metallic debris, essentially molten Inconel from the nozzle, were also found in the -nozzles, but not tabulated. Their penetration may be esti-mated from the as-cut transverse sections of the nozzles. Although some of this debris contained small quantities of fuel, the quantities apparently were insufficient to register in the activity profiles. Although porous, ceramic-appearing material was seen in the as-cut { transverse sections at elevations below the nozzle tops, such as in H8 and L6, j there seemed to be difficulty in retaining it during the subsequent sectioning operations to form metallographic mounts. This would attest to the friable nature of the material. { Fuel material that was retained at the lower elevations in most cases j had two features. First, it appeared to be in the early stages of transforma-f i tion to U-rich and Zr-rich phases, indicating relatively rapid cooling. Second, it contained Fe, Al, and Cr in the grain boundaries, indicating likely 1 fluidity significantly below 2000*C. That would aid the fuel's mobility to the elevation where it finally solidified.5 s 1 In Nozzles M9 and H5, which melted off, the penetration was shallow, in-i i dicating a quick melting and relatively rapid cooling, the phase transforma-j d j tions in the fuel areas notwithstanding. It is likely that the melting point i i d of Cr-oxide (Cr2 3 melts at 1990*C) dominated the mobility of this material be-0 fore thermal equilibrium and lower-melting eutectics could form. The phase transformation of the fuel would have occurred below 1990*C while the solidi-i fied fuel was trapped in the insulating Cr-oxide. i The fuel in the tops of D10 and Ell differed from that in M9 and H5 in i that it was trapped in an Fe-rather than a Cr-based matrix. This reflects two things. Fi rs t. the Inconel did not readily give up its Cr to oxidation, probably because the temperature was too low. Second, the source of the fuel and the Fe-based matrix was probably the same as that of the Fe-based surface ) scales. That many of the fuel particles were shards and not solidified in-- l I l 36 . ~. - . ~..

l 9 situ masses indicates that the fue'l flow in this region of the vessel was l cooler than the flow that contacted M9, H5, and H8. This is consistent with a .j scenario that has the fuel flow coming to the vessel hot spot from the east f and southeast and piling up on the far side against DIO and Ell. (Note that the surf ace crust and major heating load was only on one side of DIO.) VII. CONCLUSIONS ~! The following are conclusions reached from the nozzle examinations and that bear on the examination objectives. i 1. The nature of the degradation of Nozzles M9, H5, and H8 indicate l that their melt-off was by liquid fuel coming at the nozzles at an elevation ranging from ~140 to 270 mm above the lower head. Surface scale on the nozzles below the melt-offs suggests, albeit-not con-j clusively, that the liquid was atop a crust of solidified and par-tially solidified fuel debris that had been cooled below its solidus l by contact with the lower head. i 2. The fuel flow on the lower head followed multiple paths. Nozzles M9, H5, and H8 suggest that flows occurred f rom the east and south-j east, but bypassed Nozzle L6. i 3. The fuel debris in and on Nozzles D10 and Ell suggest that these j nozzles were at the periphery of the fuel flow, likely on the cooler far side. 4. The pattern of nozzle degradation, the assLmption of a decreasing-1- l thickness initial debris bed, and the assumed fuel flow directions j are consistent with a vessel hot spot at E7-8/F7-8 that was caused l I l. by hot liquid fuel atop a progressively thinner crust'because of 4 lessening heat tr ensfer to a warming vessel. l 5. Significant nozzle temperatures ranged from 1400*C (melting) at t 140 mm f rom the vessel at H5. down to -1000*C at 64 mm from the ves-sel at H8. 37 . ~ - - - . =. -

t f 6. In addition to melting, nozzle degradation mechanisms.were ablation by liquid Zr, intergranular penetration by Zr and Ag-Cd chemical interaction with Al, Cr-depletion caused by extensive oxidation, and i i internal pressurization causing hot-tearing and nozzle ballooning. i 7. The presence of significant quantities of Zr and Ag-Cd on the vessel { to interact with the nozzles is attributed to the prior deposition I at that location of control assembly debris. The. depth or nature of such a debris bed could not be confirmed, but the depth is estimated

l to have been a minimum of 120 mm at the H8 location.

j l 8. Fuel debris penetration downward into the nozzles was influenced by. I i the temperature of the fuel at the time of entry: its composition, and hence fluidity; the temperature of the nozzle and its ability to i solidify the debris; and the degree of i*teraction between the fuel I and the molten nozzle in entrapping the fuel in Cr-oxide. j l VIII. ACKNOWLEDGMENTS l The authors acknowledge the unstinting support and patience of A. Rubin, j C. Serpan, and E. Hackett during the course of this work. The endeavors of j J. Sanecki for his consultations on analytical results: D. Pushis, W. Kettman. F. Pausche D. Evans. and L. Essenmacher for photography, specimen prepara-i tion, and metallography; and E. Hartig for manuscript preparation are grate-l fully acknowledged. The authors sincerely thank D. Diercks and T. Kassner'for i 3 their consultations and being the sounding boards for many of the concepts documented here. j 1 I I I t 4 38 J

j IX. REFERENCES i 1. D. Akers. S. M. Jensen, and B. K. Schuetz. EGG-0 ECD-9810. Companion Sample ~ Examinations. April 1992. l 2. Phase 4 Status Report. " Removal of Test Specimens from the THI-2 Reactor Vessel Bottom Head." Project Summary. MPR-1195. MPR Associates. Inc.. October 1. 1990. 'l i 3. G. Korth. Presentation to the Project Review Group. Idaho Falls. 10. May 12-13. 1992. TMIV(92)EG03. 'l l 4 Phase 3 Status Report. " Removal of Test Specimens from the TMi-2 Reactor Vessel Bottom Head." MPR Associates. Inc., April 1. 1990. j 5. R. V. Strain. L. A. Neimark, an J. E. Sanecki. " Fuel Relocation Mechanisms l Based on Microstructures of Debris." Nucl. Technol. BZ. No. 1 (187-190), f August 1989. i 6. " Video Inspections of Incore instrument Guide Tubes". TMI-2 Technical Bulletin. TB-89-07. Rev. O. May 23, 1989. i 7. T. F. Kassner. ANL-MCT Corrosion Section. Private Communication. -l 4 .I 4 1 2 1 I I i 39 i 1 e I

,ha u a s a a - j i l Table 1 - ANL Nozzle Segment lengths. Elevations, and Fuel Penetration Depths- - i i Elevation Elevation of Fuel Penetration l of Nozzle Segment Stub Hissinga Top of Elevation above Base. Length. Length. Top. Segment.b Nozzle Base.C l j Nozzle mm mm mm mm mm mm i i M9 119 254 26d 25 280 241 l I L6 94 241 64d 0 305 75 i i i H5 107 146 0 159 146 89 max 117 min i H8 0 70 51 184 121 (64 l l DIO 244 235 570 13 292 55 max l 184 min Ell 221 225 77d 3 302 204 ) 8 Based on measurement from either top taper point or midplane bevel. DReferenced to nozzle base. CBased only on gamma scans. j UCalculated as the difference between 305 mm and the sum of the two known values. Measurements of stub lengths for D10 and Ell f rom photographs were not deemed suf ficiently [ accurate because of angle of photo. . I f i n e t 1 ' t -f a t f 4 1 40 t i

3 I e i Table 2 - Composition of Debris Areas / Particles Containing U-Zra Composition wt.1b i hoirle/ location U 2r Te Ni Cr Ag Cd Al j -l { 99/779 m firside acirle t Matrix 29 8 6 5 43 7 i Matrin 55 12 5 2 15 9 Particulate 58 19 8 11 3 f Fuel mass BB 9 1 1 1 Fuel mass B3 15 1 1 l Fuel mass 55 12 5 15 2 9 i I L!i/793 me firsiee rerric) Shard 100 Solidified mass. IC B3-87 11-13 2 1 l Grain boundary, 1 41 19 17 14 8 Solicified mass. 2 17 54 9 1 11 9 I Solidified mass. 2 74 27 -5 { H5 /140 -- r iatier enirir! Ceramic area. edge 25-30 13-15 1-3 1 51-57 i Ceramic area. ecse 82 12 1 3 1 Ceramic areas. centerd (35-40) (12-16) - (40-55) .l Ceramic areas. center 13-30 B-12 7-22 2-10 40-77 l Ceramic area. edge 28 15 33 11 13 j I gq/ m m-f i-sier enrriet i Particulate areas 60 30 4 3 1 } S!0/290 m-ff= side aerrie) Particulate 1 65 23 4 3 5 f Particulate 2 63 12 5 15 6 ~ j 010/158 * <!eceded in aerries l Particle 1 EB 23 4 2 2 { Particle 2 77 20 1 1 1 6 Particle 3 91 8 1 010/97 n teutside acirle) i Particle 1 14 62 B 6 2 7-l Particle 2 81 16 2 1 Particle 2 75 16 6 2 2 Particle 3 10 77 6 5 1 Particle 4 22 78 l 010/E9 em touter surr te) a Imbedded particle B2-12 1 3 1 ~! aNormalized to -1001 metals oxygen not censidered. i Distimated accuracy is 120%. f Clike numbers indicate either more than one analysis on a particular structure. or .j tr.dividual areas in a structure. l oparentheses identify estimated valves for portion of analyzed area. ? .i i 41 f I i I - - - -., - + .m -e.-

t t Table 2 (continued) ) I F Composition. wt.%D I Nczzle/ Location U Zr Fe N1 Cr - Ag Cd Al i F11/7A'1 em f irs t ee enr71c1 i large sharc 83 14 1 1 Small shard B3 14 2 1 t Matrix 34 53 8 3 3 l Natrix 47 44 6 2 1 Matrix 66 27 4 2 1 l Matria 87 10 1 1 Surf ace fola toutsice) 74 10 2 6 2 6 F11/774 cm tintice merrie) Inside nozzle -9 -85 4 2 1-Inside nozzle 27 71 1 1 ( Insice, agglomerates (avg) 62 16 19 3 l i (!! roc== m ter rur are) i r Oater scale 20 20 57 2 1 i[ l I f k a ? I I I ) v a r + i [ t I; h 6 42 l t 9 -'?

__..__ _ _ = _ _. _ _ _ _ __ I i i I Table 3 - Summary of Hardness Determinations f t l Elevation from Nozzle f

Vessel, r

mm 010 E11 HB H5 L6 M9 i 1 290 208 1 29 l a 283 167 i 7 l J J 280 14024 J 274 137 i 4 266 13613 i ~ t 260 124 i Sa ) 4 158 124 t 2' l 4 130 105 1 2a 108 14817 90 190 1 9 j 82 161 1 4 -- I 77 169 1 13 69 168 i 10 l 64 13314 l 38 202 1 28 l 25 198 8 0 217 1 13b l i t aCr-depleted material. D eldment. j-W 1 .i i j 4 i 4 8 i } 43 I 1 1

m "A N e e i l A B C D E F G H K L M N O P R j b l l I NORTH / N i / N I 15 / K l O !... -......!.. +.;

O

...\\ [ .. -......,.. +. -.. +. - -.. 14 1 /... O O ll O [ O ! l0l [ l 13 I I 0! O' '......L.....4....i O; 12 ) .......-..L.....4..-..... ..;-....+...-..:.. l [ i 'O 'O O [ [.......'. 4 . -.O k..- _......

7...

...-..+..-.p. .7... 11 ,..--.-..r ,._...q,. ........9.... 7.. ..-...7..

O

!O, O 10 O! 0: OiO 9 0 9 .... 4 4 4 -..

4..

.... 4 .4 4.~.-.,. 8 'O! I i O L J O! ~ ... q..... 4..... 4.... a..

4.... - 4.

...i-. ' . -... ?.. 4.-.-+- ..q ( j jo. ... O ' f 7 {

Oj

..A.._ O_ ^' i \\ i O .O. e! o 0 c \\ O O O! k O, s ...._....,i O j Ol 4 ....i... \\' O}. 2 O \\ N Locations of Boat Samples o O Nozzle Positions a Nozzles Examined at ANL fig. 1. Grid map of TMI core showing 10 Cations of nozzles examined at ANL, 44

i. a = \\ l l 1 LOWER THREE [' LCSA PLATES /. l hl, f,c( l j s \\I/d ['d l I/M [/d l '~j (/] l l/,l i [/)~ l \\ i / j#

1. f X

/ t[-. m I d [\\M - f \\ r l' \\ / = x ) I ELLIPTICAL FLOW DISTRIBUTOR PLATE / ~ 4 1/ 2" INCORE INSTRUMENT \\, GUIDE TUBE

== I s ~ 87 1/16" SPHERICAL 12" /A "A 'us A y '" zz"tE M(N\\fSAMPLE ELEVATION E o + <n v 1 3/16" CL AD \\. 62.5" T l N TO CENTERLINE h(MIN) s x N'O e 11 $Ns\\\\"NV L Nozzle ELEVATION Fig. 2. Typical in-core nozzle with seal and retaining weld. 1 i urn associat es '*";?'s" f 45

N \\ l N N N N N N N N Incore Nozzle \\ \\ (Material Inconel 6001 / k D .6 2 5* l.D. 12- - 2* Dia x g' \\ Seal and Retalning Weld h f ' Norn Cladding \\ 3/16 N 500 Series Stalniess Steel / I l [ r 5 3/8* Nom I w l d Annular Leak Gap of 1.00' O.D. x.612* I.D. inconel 600 about.005* Between incore Pipe and Vessel Fig. 3. Lower-head area and in-core instrument guide tubes. "[-r*2-3o$2s T/24/90 46

L w K , q,w gg 3 x C y 4 7. 'h f, z,3.x,. 1 _ M3 - ~

40 $.

r ') g. s lQ:/ 2 .Y a n& t. e;, + an ,.se s .h.. v. c ~R1' ) 4[ ]p1 u y 7 ./ l' .,. A i A'. 3

c w

ap hhdL L ,f

q h2

.- ?.

,i, w.

,.j R E 4 y

21

~: n 4 s u ,a ':145 (l bifh ,,,... i.3..... i.,,3... i. i... i q, 3. i..,- 6 ;. 17J. 18, 16 1 Fig. 4. Elevation view of nozzle segment M9, as received. (282582) 47 I .1

f .e

k. -

,n.m l' "'$:;4$h. ,,, m : .s r< n.; x .. ~,. y -,<,n, ., g- ..p...v vr.mv g ... r.... .i..... :.i i Top i i o^ e. ~ ~ ~ s ,,a w ' ' % n,,, 4,y g&s w ..s j m,/ ,,+2 W274%%&.. .s ,,,,,,,.,,i.,,i...i.i....i..i...ei.,i.ei...i 1 1 7 .i.l.a. 5 l.s.l.lo...t.l.s.l.a - t.l. t.i l a

.l.i.

t. Bottom Fig. 5. Top and bottom views of M9 nozzle segment, as received. (282558) i 48

i 4 l I i I ,n k g: E 1 E 6 A e4 I A V qN N 4 N n m

m ss

< E~ M N h + 00 p h ~*'i' '*~f [ $,0 h hs h h k,) ?. N. h q ++r-i l m u 4! \\ ~- i 11 01 6 8 4 9 s y g g -g, e i e i i i i g u e ) OC& W 3C - 01 & 2.* ema - 05 Sam vac o,0; - 0c a i 3 "m 8 CC ~ 0V 2;- -== - Os M "u -m-C VOM

• 09 C-O 9

C - DL \\ j CEE - os e:S "*3 - 05 53a - 001 - ~+ s en - UEs - Ol! oE .-u B%- ~ 051 323 6 j - Oct (seyouq) uoqqqsod sa Sqqaqqog ggt _sg 30901 4 0FI f w 49

) t hg i r v y ; g? ( S ,?j ' r y e .gQ e t g n ? e g+{ gM c g e g M ,y h yni e p .. ml.b i ,lW t iw' O ) p'[Jj(vj f. S {$ s t ef a g4rf; l[!1 j'fsi n d i; f h' 9, . i t a k ) h.?lt t l f e l .vg9L ( 1

4. ~

4 re k i t tn e .= c e h t r aen 9 M e l zzo N ,Q, f s

y s+ ( - - Ny,/

o v p e o t h g u - ?" o t r r [.' h t t) 2 n .j~. 1, " T, u s8 7 n6 o0 .Y" f. i8 t2c v ed sn a n-l a3 [+. n8 i 6 .[ z,'. d0 u8 t2 ~ i( w .. 'I' .i-g n oX ,. N L% L2 t c 7 g i F 8 1lll li!llllllll ,llllI l, l l .llll! l ,\\l ll

i j ) m 5 9 6 .~ 0 8 2 g:4 ) X 4 1 o t .,,y49*f. + d ecu ., ) - ~ _ j d e 1;- r g,'~ g X g 5 'f i,, 2 g e .f: v. .t .g'n_ vy ~R n/,~)' t a 1 i g, 't ,. r'. l w9., sY,;, p%y .J a n i g i f' r js - -.+. O .% j,., a + )T y ( { x t .t' nt _.%',e n '%'f ..p s 9 .e* ,j 3 M ., *$ >s,; .,%hh"}F'fkv '$'a,*;4- ., ~,. e l

f. p.'t.W:,'s.i,[gd~&

.\\ z .. %.',s $' y- ~ z 2 ~ o A 8 S N g' g.44 4 l$ j

c. % j',, - }'.Q", ',M

, T. f g ,1 o _4.2_'4 . g si - i'( p _Q l o g. f '.,*' t r. h ,w #- ' g uo +- r h t t ( no i x. t c y e s l a = q,y,$ n 2 i d

s u

,f j t @ e. g i y", q, n f o L b y i 8 O g,h g i F g i j; l l l l l

- = '*, /. r --) Typw ; emn e.e ppqg l p: i-c- .,# - ";q l y is i -; }3 [ .Q-4 l 7: j._ ' 'A M.* h' k,+ ? i l. (- -[- ~, l o -9 4 Y ' ( .] j T g. h .:' '] J ?z;eJ^j'h/- b.. & ((jl e.i ifN.,;. { Qf?f!?... A ~- M. 7 J:: ( i' i 4: f'- 6 1 g g . *) %., - ( g a I -, ( \\.. - g) -]. 7

• 4 6

e Li 10 s l Fig. 9. SEM-BSE image of multiphase fuel in Nozzle M9. Light f material is U-rich, medium is Zr-rich, and darkest is Cr-rich matrix. l l l ij l i l ?- U l l ? l i i I i l Fig. 10. As-cut transverse section at 241-mm elevation of M9, i l showing metallic and possibly ceramic debris between i 5 and 8 o' clock in the annulus. 2X (280685) i 52 i i

i l 1 f f i t i d h .e.p. ?'? ',{ I d,i ; i m f Ve, I ~e. -r k -. xv 4 # ,r nA

i.. '

y 8 k y 1-,-

• {

f .z '.w+f: 1 ...g. '[,. .1 g. f -g n:

r.. -k 4,.

,a - .6 %, "E, ih .e.., ': +% y 4 , 'r< M+ f',' ,n ?> m..Y_ 5~ ,. 4.(Se, ,( .\\ . o s.. r .g..,

+. 'i#.

s se e.. i s ,,_= fsp #. i m 1 Y.n J l w r

y. p*+.

I i .s::,J;uM b-Saw.,IS. 3 r \\ ~ J 1 r.ecep3v.eccper.oncrev.i.i 15 4.14,.1.7.3.18 Fig. 11. Elevation view of nozzle segment L6. (282581) 53 -1

i h 1 L:;;f;__3_y e45 paiappejappeippegipppivre n.l 4.. rat.va.1.J-PL.1r.a 1..;...:..p o p t E .- m 1;.a: Top i i I n '.*i e i C. i appp'

pg Up p; s t a plignin gs t e1a p p p gi t.....

1 :.,. .t.. ..t Bottom Fig. 12. Top and bottom views of L6 nozzle segment. (282587) l 54 {

i i i l i { i I I f l E AS Sw s m o I n- + a <o j ( FC0~ % o n ) q N N h 4 T T _m o r i 4 w F i _. z y y l j y Fr< 8 -r- - 4 l e g 3 , '.f,. b- - l 4 + / ~.i $E I j e r o < :.._. s o 6 ? f ? s y t g i g -o ? l - or l C - oc E i a - or x: I - OF 3 I U s J - os E O - 09 ff, o 3 - OL m - 08 1 .T i j L - os a p V J - 001 l - or I i - Oct t [ceyoul) uo111soa sa Raqaqqog gg7_sg 30307 _ ogi ~ i 55 ., -.. - - - - - -.. -. - _ _. ~... - - - - -....

l l i l l 1 I 4 f i . 3 y\\ / j a 4 j .. ~ 'Q ' ' ' ' 1 i l i

l 1

i 5 l l I i 1 i l 4 i l Fig. 14 As-cut transverse Section at 283-mm elevation of L6. j showing a porous material in the annulus. 2X (280675) 4 l l l k (- l i i t t i i I ? 0 i b i 1 i t 1 56 i 1 1 1, F

l ~ l l l ,.[ 's 5 '. }* i .e -{ '. ~ t j l l i l h l 8 e l 1 l 1 l I l I e l e off' 1 e l ens,m;.u' ) l + e l 1 9 i i ) l Fig. 15. Instrument string and fuel debris at 283-mm elevation of L6. (Original at 25X. reduced to 11x, 281570) l 1 i 1 I 57 I

c a. n -

/, v b. 'M

• s.

,je ~ 3i ~ ;Qfl$f);'.7; ? .,,y, r: + t ;.gJ:.: aib...;hllV ' f":y ^ ;n p;;; & :j. }J: nj;c .,u -;y ~y y;;4* p...y .m,,' T _c,p. I -t- .y 9s.[ 9,, N k :g I a w v 2 ei ,l >' '? !k4l., 9 A' . n '^.., ..e p e ~! F y-a ..,.,,; t q}:/q:;3 :,<.. l'fy.>y

3'._J_;g.-Q _4;(,,

fy p, 2 m s .r = L. e5, ...~.s,._ 4 s: -y m.< . -- :, %H.8, Q{C $ l*lfk f,< . t'l* *li ~ 1 r;.~ x; - ~w " ~ ,.,;;.,f ,r q,n. .,4

e..

p 'k Su, '.. .+ : ,,, 3-we l ) Fig. 16. Partially transformed fuel mass at 283-mm elevation of L6. i ) a

l 5

i ] f 1 apc - 1.. p. t u ) e#(,.. %,

;;e.

i b .. 's f ' + \\ s + I j k Y: -s '~ l Fig. 17. As-cut transverse section at 77-mm elevation of L6. 2X I (280680) i t g

m...__. _.. i' 1 1 1 j 1. i {I I r., j .a { r _s i s. fT s M e ys 4 e, py ) ,r. a y :, .. ? q l -j i I s-L.. j w f "e, y .I. k. / 4 i s-a i 1 I d i I a l ) Fig. 18. Partially transformed zirconium instrument lead at i 77-mm elevation in L6. 250X (281664) l ]' f i .i i y.. ? 1 o>, ,a + 1 ^ s i i i ..s-2 4 ~. - -, :*.= # i --.N .~ ~ 4 4. L ? i =& i i 4 d I 1 s. .e i i ..+...,,

v l

r .p. s ~. 1 s , r e, 4 j 3-l ,J p l Yr 4 a l 9 s j p e j 1 w . ;s, i ~ .p.-n / -t. y..: { Fig. 19. Etched microstructure of Inconel 600 nozzle at l 77-mm elevation in L6. 100X (282531) i i ) + l I 59 I 1 x- - -. ,,m.-----

AG-1 J-2 m +. + - -, AH-i b .sw -i 4.a'f, 6 w,, %,5. 4,, i ce2 y. e. } .k 4 ;a v .c,+ ~ - r < - ._ 3 9 f )'JtQ ' ' 44Wjfa%"' p i a.,, s:. A,v,.- t e a (p,% ** 2 i. ,s u y t O!h'{. c6 ? g % if syg%y ,sd k &3 4 %r:;- m:r n:0 ass. I x4 .-ffr[W; .c . v% ' ' b. ay i b { 'y -N ' NA

l12

,.l fjg[]iy '[ *

a A,.

l w:o %:7 gy upf u4 u,g s%. g.r ;y. y ?.. m g, gr a - - yt. i ,V V ' $s ; i .,m,... i fq ' O - e. N .,g , Iv.f $ r g$ Nh'hetk [. p ea .%w --,em ns m x I'j8}'ll'8l'lIl'Il'l'{' l3l8ll IIIl'ji8l8jil8h8lI{#li 31'j!l' l .j.l51..1 4..s .1;7..:, .1 8.. .11.9.. f Fig. 20. Elevation view of nozzle segment H5. (282580) e e i i i t I e i t 8

I l y,m_ ;w 7q; p,,- .in - m. L. 9 h-1 x. 't: - t s g -- %n : wm. - .i...,.i..i..i.i.i m i.i..i.i..i. u 4 i i i i i i.i i.i i > i.i. i..i. 1< 1 7i 1 an. 5 o.io.lo.io.,o, o.la.io. io.uo.l.,.s.1....l.i.f.17 ~,,L, i. i .;.i.i. i Top (stereo pair) i i b 7- ~. .) g ["' A i9 gj ,n, 1. bg. x l,' ' i ec $P N q :)-Q c .ep.y I Bottom Fig. 21. Top and bottom views of HS nozzle segment. (282585) 61

~. ) i d l i i l ] 6 1 i i 4 I I I

SIh, j

7 l .,s.,. c i Fig. 22. As-polished bottom end of H5 segment. revealing only a solidified metallic mass. 2X (280533) i J i i' i i i l s I I I l 1 l 4 s s 62 l

3 E E E 7 E E o 4 E O g ,e g ~ Q b f h g y a a e T T t_ m {~ C ~ FM i Q i ,g:. ry .yi . mu. '::s p - e n N .t e.,- % ; 7,, R. - - a y ,? g W o 1. A E: 8 G P-hT m a 6 8 4 9 S F E E 1 0 O E i i i i i o 2 - Sz ~ O - 051 c 2 - sce og SE - 00t 5a i - S4C E"5 i cU - 0SF S5 l u u- - Ses 6 7% -009 m I o$ { - S49 E ', e* - 0SZ ag i Du - ses

g l

s* - 006 gb N (seqoul) uo111 sod

• S ^ fi11^110U ZEI 80 10101

~ S'8 o-0501 j LL l l 63 1

I I i ,j' Q p,* ^~ J w. ....A M.. $'4.,, 'l g R QQ% r ,c p. m$p;,,.7s4, s t 4 v 2 Y

.. % Jr~

g 5%%.s-i a ~~ l g+ } ;; ' > TD 'f .:~ ,, >l %2f l p.gS}f n. r Fig. 24. As-cut transverse section through H5 at the 114-mm elevation. l 3 2X (280530) i I l 5 1 3 4 i h ^ ?! (?,;*0 .g f){ ;tf'"f. ^ a; ~

g. :.,f l

f) ffr a,- l + d yg;.. l Mr r ,-[ a t '.,

• O

$${ - v w e e. 4 4 -j j; 'g. ~ l i Fig. 25. As-cut longitudinal section through top of H5 segment. 2X (280535) f [ I I t 64 i l

9 4 5 -1g W h se 4 .5 1 t. i x 4 ,I T p ' t< Rap-2L3* L ~

o..

l We. ,A.' ,+, oy9

a. /,

x e vp*' l,

W e

b ,y# M.,. y ?, ~~ s, . a_, ;. y, 3 + gh 5' ' h.' 'f; . 4 - p.M %W,d- @S%* ' p , fi %"I - .N

1. f;k,\\,p~'

ff&gR.p, e l& s? R -)g i

• F ;g-Jiip 4,.

33 -,g y. yh 1 4 3 f (./-qq "q +4 l7 r ff ., ; EC Q' - {D.,;ukb d \\m,j,...

n. :;..g. f,s, j.

l i q p Lv n s:

v. -

h R*;,,-f ;, ., M-n,,,, g Mg k ?f.vg3 _m i 3 p s. e ..yga g,, p

-+ m3 j

i,p,, ,- h 'h Y.. " x&: _4 E$2i?&.:mmQQsf ,. [e), j : '.,, t., 5 % w... ~ .b < 'j t wgr ~ a c$ d,QGhur-egyb f;y h, 'o e - + > lw p ::%'Ds' } 'p.:t.k: ~ ry y$i~,,,', ; % W,,.o T ! pp#9.84 x ~ 64.y;<j I. 7,. 3 t h "' d q w' 7 3,. s / gyp..g; s- +, n -

4 Ns g

1. 5 469*fe.y/vd.,h$pW%Q Ne y

g sk9 am,[a;d zy Nl pk(w %c);yj%$ i sif4 V, 4 g> n . l;& }( % Q a'

. ~..

':,'ay A g: Qh .y i y

• (f[DM L

T.L i';. \\@,$[y.$ gyy jf@Y l j. f. Ql' g V " y h, e p.Y {, /$ l 3 D )k (9.'y$5) l b -- J Ih ?S!q'g,'$ : ?> _t e.. 3. p.h?k~:- I DNb 3 1, * \\ N ^ '.?M) 4 f Fig. 26. Metallic and ceramic debris at top of fi5. (Original at 2SX, reduced to 15X; 280693) 1 i I a b l i i 65 i

m. i il l y P ..-. a m . 7 y$ ..y vy OQf l,ll ,y [ p n :r : +C~ -. y~ ~ .p.s.s. W, -?- + .Q... c. rO . s. ...a ~ v P m., ~ -y. bM,,%,ggyp ' 1 k ag?*"y i ^ - ^, 257. f 7 - . w -2 e. < g' + 4 4 g-* n_.:... :. , h 'k ^4 ) 9~ ?, '4 l*-w; Q, s;?.{ ' + i.<.,,, % l* ' ' y,' 8 'k y}fg -1 b-

i. {

.a l ?. iQ If l[f y, ' J r 3 '~ g? J 8 ....f.;.-x .p. L%h c ~. e - _n,.,- m - . 9, ~, f.." pA ;"p "'9

i.g ks.

.'4. 'l, '4 - e 4 = j Fig. 27. Microstructure of debris at top of H5, Fig. 28. Chromium-rich platelets precipitated in showing intimate mixture of U-rich Cr-depleted Inconel. Bubble contains phases (light). Zr-rich phases (medium), deposits of core debris. and Cr-rich matrix (darkest). w. ~_,.-%--v --r- ~ v.- ..s-.r-,-- c~. r

---

+-,i-..+

..-,-.-.mm-- --.o.. -4 .-rm..rww-

. ~. l l t l i I i ~ i i l r l ~~~_N I l N. ,J ' w\\.._ l d Fig. 29. Instrument string and solidified Intonel mass at the bottom of the H5 segment. (Original at 25X, reduced to 12X. 280635) l 1 i ) i 67 I

I 4 l 1 w. g I 61 l j i i i 4 ~ l j i l O J' O s W k { j a ) i (a) i a I i i a l s, D,4' , s i

• -a i

i e . J.' .. 'M 9 c. s. p Nk f hf. i Ay;, - k...;L L ? ~, - . a wq). ,;4nP% wj,;c~y,g& 41y.,g,,,.%,;,,,-.g"

p. 6 m ;4yw n

.v-, 3 x. l tese.w ay# g gg.

,4.,,,.g 7.. g m...

s. 7 m:, wq N L hiG'?!hffl % ? i t t ) t l (b) I Fig. 30. Shards of Inconel 600 (a) and fuel debris (b) within instrument 1 l String at bottom of H5. 250X (280582 and 280584) 1 i' i A

e e A' TL' : v. C '**& * *

j..

d,

• E,y+;3, %

L

• uf&

+

• ?.. y ? ' /, -- s' -

r < n}4>~s, g,%kf. ' ',g y'v.p > A, < / ;[', r,a a y % *. 4 ., 7, . " fj '

1. d',,2. ;", -

y 3 s o- .'t ~- y. sn. "Q;'A a ..y < f, :s. e 3 -..-+Y. . s 4.,. y 4 xa -.Lj <. Iye n.* y e ' 4.- pr,*,

g..

.r . - + - h*3Lv f j A'&' 4 (y y ) '* h.

4. # pA,f

.+g'4.,f*h .n(a4;f Y, f, (# & * - f L- .bn A ,,, S*%.W.&.3, 9 y l n &. rg, - y e I-. d ef 47 ; y ) % d,ek.,[ } 4 CpO>'S.., (,* n. J. "' s,.. w #,#.,, g" T,Rl ~,g7#1.,,f + 'j. *

• y,w

%. r. c.* ..e ~ fl# =- .s ,,4 4 - ' e ,s. n. e p.4. rA.- p._..*3)%V f. t q > Q:* ) p % h* - +*.. \\p.,~~ < a y. .o c.r 4_ . pt 'h? %,,M n.p V;;*:%l% g>h ~ f AW) Qj,..)+% m rc' '! ~ o.4 c,%^40.s A 4 > r

• ., l..i, s,.? '. 5 D ~

%U $v 4 mr fdf 6.g ?.ag' %-.i., *,,. Q, [= f ?/u +: ./ y ~* g4s* $,g C 2 .-4 e - . ' n. gp / ~ 3< q,pe N" : *,d; (f- -4* s. =.,, 7 ;,/. -L f.,o - a 4 .F b y Ls a; ',,..i.. 4,, - " ;, >5Id g.

7. n 6~

'ss 4., $ ,p e ~ Ar f 3 ,,, n ' 4,y;, % r v+ w'.

• h ',4G j., f

y. #,,

4 ^p,,,., r 1 ' =- 6 fp *, ; y[,,,, -), [,.C f, _ Q. (f f b

• g'I~,f

.,.y J ,~, u.. f,;, f 1 ^ f.

• $s

.h..,,

w... r '- ' ytrw e

._g. 8 / +,# ,r e" .a - s h 9 ..s i 9_ + ) ' r :-,. Q'.< .. a. -g. FL* a

U.

+p -4 3 ., 4 ;. mg

4..

e ' qf .c

4., <.

3 T ik,: ' + u n. g... e ...u Am *+.. yc .4 m.g s an n 4 , 8 '>. n. f a : w., '_ ?n. _ i% .., k

Q, C

NQ * '" %f7 M; ' ;y V ~* 3 , f*?'I: "; Q _

• v;

.y m, r yh', n' s , ;/h. . 3..a dy'. e ne J s

. o, ca.

m a ., A;i.- +;-,,' n g .., g l e. n - : = q-v .x {p , mq u f- ,,e J ,,,ms m ;J;' -w..m/ *m 3 jr ~.. ' 4 % '; '*Qi;, y+y <, u - 1: ,.9 n*< n

?' f e.

. sG:. I a, < -.; - y;;AJ, (c.{ [, y# . s~,. a;.. -.h,w. ? 3 g q %... - ) 1 ft. w L },. .1 g 4 j'

. m

~ x n. ,. -p Gu _ rpl 3 8.((k s 'fe. (' d N (c 97, =.%. - Ia -x.,+ .,m.f

s. w,s *

+ e , 3,',,' ,- af s s m_ 9.. e g a. s -+ v,~. - m... cs +. + y i .s A, .I O j i Fig. 31. Bottom weldment of the H5 nozzle. 9X (281587): insert at 260X (281635) l f d 69

P [_%, A p Jl.'Y / s. .K, }Ur'.u ' 4"; R

1. +t$

a.q c9[j* Top .15,1141w.v.v3.vi.ni. .t.i v cce. p .17.,. e.)g ~ j,.. - 45 l m-a n =b l" Side T i L': / x...

x; L,.

.pe, - y v }, g,I). # g 'i ). j Fig. 32 filt - Ih - c: ? ^ Top, elevation, and -p;q,pyqii.pg.p,pj,p.pg.p ipgip pg bottom views of H8 nozzle segment. 1 -y , o s,I.- I o. ..I. (282586) a aw x. ,;,yub "'fD a.. 'y , " J.%g '% TUkC 'S. .e;,:. kh?N$?hik ~ x %[ g>f,f, b. fi. M. 4~ . xdM Bottom s .ajn. ' ' ' g +., g,. " + %_ h l:,, *.b .-+ '~ $ $1 ^ b / ,,r..,....,. . y 11 12. 13. 70

i J l i l .= g e i 8 426 cM 426clB 8 -n g . e 2 e.5e. MG' 1 t 4 i c 426Cl i s t g E 3 G4mm lA U, 426C2 + ~~ i l a4ag"aoasaAgao Ieiiomv" i'"'n'Fi'ii 1 7. 18.,.15 2 2 = - ^

• 426 cab 426C2C I

Fig. 33. Gamma activity profile and sectioning scheme for Nozzle H8. Location of longitudinal cut shown only to identify specimens, i not actual cutting plane. 71

l 1 .\\ - t ? 1 -y 5 i,. ) h l ( ,l b il J i 9 >> k., f t I / h ~ k s, Fig. 34. AS-Cut longitudinal Section through the top of H8. 2X (280653) l 72

.. _ ~ l l 1 = 1 t .I i ) .,7 =e d. 7.;.iM M @;* a. .v m ,,y 9 ;. m 7, s i .g i l i i A. i d 4 ) I 1 1 l' i Fig. 35. As-cut transverse section at the 64-mm elevation in H8. 2X (280652) G O m I i W d } i s 1 4 1 1 73 ,n.--r-

r h i A ^ \\ 'N ,m- . J '1i y- ] j a \\' 4 .Vf'(;- f a N, .[ -q ,..Mw r. d)>, 1 1 l Fig. 36. Metallographic section of instrument string and metallic debris at the 64-mm elevation of H8. (Original at 35X, reduced to 11X, 280453) i I l 1 i l a j i l 74

'F$ s v m a r e-M I - L + c y ,? ,L". ( J ) .A. { j 9 u,, h* ^ i E l g sy p p j x .P l 4, V " ' *, s **h. N-d ] Fig. 37. Eutectic structures, containing Zr, U In, Ni, Cr and Fe.at the 64-mm elevation in H8. 250X (280462) 1 I 75

l 1 i s, ..; - 3 I Fig. 38. Ablated surface of H8 nozzle at the 64-mm elevation. (Original at 150X. reduced to 56X, 280733) i se t a ,,n 3 4,, ,,m..x,;. t. 1 s w.s.. Ss E g. f 4* ^ f r2

q.. '

e 1 .1, : .-4 e f Fig. 39. SEM-BSE image of Ag-Cd particle, ~ L. sc" f e; e and Zr-rich material penetrating 'e-a surface of H8 nozzle at 64-mm elevation. s. 1*%. J .~n g 5 3. S L. '%g,, { t N .:S i t

(/.'

t l; '7,0 l? j QT

1. J l

s t ..w,-,,. -,w- ,,,v>.e m--n. m -e.-- m. es- - - -..-~-, -- .~n-r n

• --w

-..,-.vm m-- .w-m-- w --,-e-- , - - - ~ -., -- -e---w--w----. - - - - + - - - -,.~,--e .--aen,.,,-*--..--- -- - -- - -me

A kh3?nM /s[w&.,.yn!y:ae'%Q) m t i , -g s.m;g

• #*1 s q* s sp

.; a. 1 v

o. -%

,m W ? My# f %ptQ)f%j;i y% Ng '.;,.eM[kM -j. Mpy i^ - >:j g,.s jg;gy 3p % v 3,. w ty a e. c

l::lj AN ?p.'1y.. fl' h u,, qr jhe.% ui1, j tu;

. 4 n um-aw q)n . - n,2,<9;g 4.4 - .,P

• i A-

.. g a Qg - p p w so~ .sg 3 m :. p -gayv s 2'W1/? Qbq R Wf M q& j.,.A'+'t.,. # s%gM,nm. e n : m,

7 w

m,a , ~ ms m e. - :~ - - * ' sp, M. i, # 't ' + ., -. - / r 1 4 m.r-g 3 .--f([*5l2 h.4 4ylf,[ A fT a m ]PJ!,,. ; .. # ).+ f ,.?.r. -ti me:w . g ) } Alp, .Q :, t"ldp g*ty. > = \\,-

c. c i '. %,.'

g,5, i '*4%.,,W N ,ur- , :%,U 'e q,sy'(*k l,1[$ } .,E ~ Ap[g n [2 ':.p - 9s

m.a +. ~

.~ r ~k $ g r lIl* V i ;'1.,g.,f*/ g.[t)A ::}' Le . 5pf.?. ..fp

• QM+);

.p p.j

. pg

r,

.u 7j w e-gj g; w m 3y v a.e , <A.s t$e. A. 4. 1 ~: --

• s.=

e >y - g. Gtkv?-f"'gdg , gjgg gg T& %A

:k Til l l

?, 4% l ~ 4.c, c ebo4sy.u;c.. u.#M n + s. 4a p, yc..,, . c.,, f. m' [, 7__9. g. y$$ QfQg-c c. , ~, - -.. m _ my g, m. ', ' ? ? '?g ' .S L u '%_c 37 n ,.i. .g ' : nl%{' (Q J' tyt,:W M:.. g%s;M &pf 7j w .m. w gy

s' w%q;

tg, m.

1 e p :;. 3 M M, ml % 1lb ?. , 9l

• a[

n 6. ,x p ? jr 2 '4. s - U}k: M Jf}*k'd!'j'I'it'j'I'I'l' l '{'it!'lij'll lijf.P *P }*l' 17 1S 14 . 1ti i h6. Fig. 40. Elevation views of D10 nozzle segment. Side view shows crack in nozzle surface. (282578) 77

y%;u y$ Mf28 gl t ,, e i,,,,i.o., ..gi.pi,,,, p i,pe;,,, e i,, ,.j., p,,,,,,,,j., 1 8; lo5...i.,a.17,a,ia,ia n,, a,,,,,,l,,a,,17,a,n I,,a,,1 8,a,,,l,, ...i... i,, Top (stereo pair) pa"J'Q w.. e .ses m 'g y 't WD5 - we, N, ,,,,ei,,,,,,,,,.N,.,.YR.,,,ei,,,,ei,,, lo6 17. .1 8. Bottom Fig. 41. Top and bottom views of the D10 nozzle segment. (282583) 78

I1 ] t i m m m E m m m g 6 7 5 6 4 7 2 2 1 Z B. l 2 3 A A b S S 5 i A F F p 2 F F Fj lF F G M G 6 6 6 1 2 2 2 4 4 4 4 b 4 4 B

i. y

( [: I F fl '"j G r 'e 4 h' c v. Y' h -l,h [" I .-s g ,x 7h. t A n. [' y, f' ~ [E $' {' I F ..g 6 s 2 4 g n s m s m n c y t S y lno 0 xt R o 1 n D w rh ose f n w i A t a eul c mcp e a ? hl g can sni i t i E gdt nuu i t c ni i 8 o gl i na t ou 4 R cl t e c sf a o 6 E d t nno /" i 8 et, aon i l as i cn f oe I $ oL m r i c .c p e yt p t ns i e i $ vmy i gf t ei cst m ).u.* aC s t ). 3_Oao4 i 5 a n ]G55. - cO, ). M [ . C> 0 o ee C C E al d mzi

llI1iil!I

!I l!lI

,i !i$ mz a oo Gnt 2 4 g i F M l (,' l

1 l l m t. n e v lz z s on a k's,! 0 1 pf D e yag h t .i '3 [ f r o 6-p = o t e h t h g u o o r h ~ t n o i t c e s l a n i d u n t) m i9 ~ g4 ~ n6 ~ o0 l 8 2 e hd tn )g. a f o0 5 jQ_ s6 e0 d8 i2 s( o wX i T2 9 g ^! 3 4 i F l,

i l

ll Il, 1 lll

i J - -s ....,>

• 2; e

s )_., ',t L *.NZ)),:3.Mi. . (i y;~ yp* %..t i

. e u

\\. ?r. w. *,. l , F. :) ~, j'7 % c, j .v ;

w, s

,..,s, Y ^ l .vy l..,,.)... 'Tu..

f. s., +,. c ' IQ },h,. -<..

.,. + t . O f.h +., - ~>v s .y. .. ')[4 v.. g$V..., A, w;- w g'tb41 ,%- t.k?!6$&? $9'Ns$&a:, .,s,,;;

e. ;c. ~ = V,. *gi,,.pp

$e p, $$tY.. E .a: .y m....y, p,yg ,., qw mgg,, ge af, q 4 5-

g);

l Fig. 44. Typical area of fuel shards found at top of 010 nozzle. l i e m.1 ? 4 1 p_ R g,[. ih .A u. 0 Fig. 45. As-cut transverse section through 010 at the 266-mm elevation, showing a metallic and ceramic debris inside. 2X (280641) 1 81

_ _ _.. - - - ~ -. 1 .l l 1 m 1 r. s,.m , 7.- 48 . gMo.%nf;; l ) b;m,b;&,=.qy v .= N 4;. g ~f 4 @ pt g# l,- e' c >: l q 'u i j .g - + gr j 4g * ' Ny%g 5.i i ..g. m.g $ w*, -%d l 4 M. ' i i i I 4 8 i 4 Fig. 46. Surface deposits at 266 mm on Nozzle D10. j ) i 1 1 . e s' i s'. 3 w.,... I ,_gyj:f, 4 $ ' -l.S; 4wy32Q/9 gi s4-w . q;7 -e t e ^ l 1 'Q! { r 1 ? 4 1 f i Fig. 47. As-cut transverse section through DIO at the l 177-mm elevation. 2X (280644) } j 5 1 i J i l I i j B2 } i i 4 6

d i n w:u< ey... .~..%_.. ' + m w.

• 9 %,p P'

%.%y,.. : < f. 9' v(Gd 8 p

),

- f 8; i ~ g g

's3 4

./ q r .a f,I M. ycj j t I i (d;) W;? pJ s .;+ 1 v iA,# 4,D:' J. A gi e,4 e :g g;iOy 3 4 y*n,eyg.y .g+]j ,.N,_.:,..c.f f j i d 14,py 4 ,M,'

g.,, a p., ;

-Jl} Y b : Y :. x., .a ni e., - k.3,. J.%?) w. l i Fig. 48. As-cut transverse section through D10 at the i 158-mm elevation. 2X (280646:1 ( o 4 1 J e r 1 i i I a i 8 J f: 1 i i h e i l e i B3 r

e 1 i i 1 t-i a l 1 QWs : "} \\ i ^ Q, o l s. i . ~f i -->\\,. N f r I [ C L i k ?. l l' kh / i Fig. 49. Area of grain boundary separations in D10 at the 158-mm elevation. l (Original at 25X, reduced to 12X 280688) j l I l I t j i i I i i a l 1 i i M f i 1

t ~ 4 s } g n i w W o i hs se l 3 ,c ni ot _ h. ir ta s ap v ee I l t . y ) ee > A. b r mc ( ms ( I i 8d 5 Nk b 1) z e( (:j, h td n . L], ta (. s a 0r

• . g, f ' tn n

1 e Dg ni i r t ss 4 t i) sa o( p es ).. da 't dn Co i f. gt Aa \\ r ftoe 4 n ) se a ep y ( l pd y mC a-xg / EA 0 i 5 g i F g 1i e i;

M e,y, -f

• f.QV D '

90 w 5 m\\p%s, p p$,uh:xwdn's' 4

.824k y

Yh*g: ggs.9 wg -w% n m.pd5~fdiTM[w g;.7%(A@M& Nby.Nb I . I.' .rggvu. a o QqM;y:.4xt.h.,x ywr: .uit C V s t.r.wu,q, Eg $.wg.y!bn, g+:', W u.-A%6m u i 76=..,y. r ?p. S c %< f s: ; g g, A.,,, ps. v m.. ~ c,* . %y;<:ss.vX M y o o p -lvp .w,,,

h. ~s:.

p s .c .e R&Nh. W. ,a , egg ~ L* uvs .c b ? . *:! F di o y$ ' sv * ~ o> ~. a . ?- W,: :;,. G.v

u O

2c 4' .% ?id '.'l, ~ ' ~ , ' b.1.2 g E g " CD 'm E e4 O V c-o e. 3 s -k. h A

s.

• 5 8 + M g:+; s$'

W W- $ I M.' e.- C k g 3 ^%. r E M44% QR hb-gf?,C ?f.D,b ~ %} [. r q ;i:n; A 3W g l8 $,- I' b h;. G k'[Mf,. dj, D 7 a, w;.. ' e; ' f ',4'. y : + ap + j' i q, e 5 y s-d I i

i 1 i qk m q.' #.; r;y; %,r, r,r.,,,;,., y._ r ..u b, 9.s N.. - Ac., e i J-wg g. J:: pp , =p. s 2. ye a:- .. 4N. -A , v. p.t g - ~?a %n n,.a

c

m.n, n%,. gi,y^ *s ;.h;p& " L;;.,, p H,.y ;;,-: M y: r; :, v.

m-

.. x. c ( n .-jg, ; mj.a eg, ,,:. a r. n f.' %v,2f - %, p p+; ;. o.~$ 3, - 1' [:,,,44.. N p/g;{, :da- .n ~

\\ bj )

{M e v.d rg~, e s e wg t {

• 3 7.

e a: x . g, n >. . - y 3,r.: x. lw's x $f -' ~ [ ;., e + f. t ~~ t'. N : v. ,j ,g .g ' ~. &,( l _$f >. ~ tw ,A j ~, f.,.,c n'4 - ..g. q 4 . il .qk,*? - ;..$lmf : I. g ~ :+p wh ,', w '

• f y.

.g ,; : 4.,9 ;., - + 4 ?,s c< 3h : ' ', w. '5 s 4hm .p- , cf g.. 4 ' r ? i Fig. 52. Area of grain boundary separations in D10 at the 158-mrc. elevation, etched to show possible second phase and internal grain structure. 9X (282558) i f l i r P i l 6 I 87 i. ~

..~. t 1 1 wt

ls' i.

3 3r .C..+9 2 i i, ?he r \\ A \\ s-jf \\ 3., %,*g s g[;;P .,p m.., i \\ - w -J- ,k >.a,;2 1 O ~9 . dt ,i;;- p '#g" R ', o + <' ~ \\ / s r ~ 4 \\ s' . [I..hjj S((O jk l \\ \\'

• ,y r

A w \\ sis.f e ? r; \\ - W~'y, > l+ \\ n ~ ., *p;: e ^ ~ y,. 'l. fu. i: i ' + ['; \\ \\ N};;t. \\ 4 \\- k \\ i 'x \\ M \\ \\ \\ s \\ s1 \\ \\ \\ \\ \\ \\ \\ \\ \\ \\ \\ i \\ \\ a i Fig 53. Portion of thick exterior deposit on D10 at the 158-mm elevation. 4 A fuel-containing area is on the left (arrow). (Original at 25X. reduced to 16X,.280694) i 9 1 i I l i 1 i

1 O. ~ e n, ,\\ % t i .s ; y

ti-m 7'

.Y LO ~%l .g y .~ l. la *, ^ i Q'. + iili:n2 c u. Fig. 54. Examples of Ag-Cd in Inconel at 158 mm in Nozzle D10.

i '"*'.',',pp,*,@')l.7 5jf^ (,', " e. 1'. p,e' elude, f,s ' w rf:\\, W k {, ? ' 4 $) l' c's .; \\. _., %.*. l). = 3 4.',,,a j i; ' ! y p?.G'f., g bQ,g y 'f tc w 's {

• .l,.,

!. lf Y ) ?"' . a. a v.. p(y. [ 3',' pg> U - s.; I,f fMf>[fj,, t \\t ybv:g; l Fig. 55. Segregated U-rich (light) and Zr-rich (dark) phases in fuel particle in a deposit at 158 mm on 010. 1 1 i b l l 1 m

il is i ) i B t 0 8 0 r i i.? O r c:e, A' 4 $;3 .i .C O O<L Oe.t - grQ,/g .m gr .s l l ,e ~ .g~ g>s#g) x l 4 /Ap 4..

~. 3 r..,

. l;p. ., :%c,au,;;?a# I s~y% a j, 527' " *2" l % % $9'?n?i. [.. J.,.,- '-..w,a**j i 9-i e.4 l %, p%,. & &!B* b? :' l ) ..q 1 l Fig. 56. Instrument string at 158 ma in DIO. (Original at 25X, reduced to 15X. (280673) { 1 i f i 1 i l 3 4 i i ? I r i i a t i 91 y

=. l l \\ l I TFi* I.sI59 ' ,c - .z. ^ s" kN ,A 1. i l. ;." *, I %. ',. +,, 4 4,I Q y'W jy _ E;h 9. v$ > :- ~

1. 3 ;;ff gh f

e x' 4 .? u, A A .k. 1h 9 c -; s. f. 6,. ..pyy. m. f 4'. ?g .g j ' h.b $- 1 g e A.

4%5Q-- :...,;,1%; -

^ a s . Q:ssy, r - ). 9 i $x.Y 1 .m h' t J

l 1

.s 4 A. ~ [ 1 1 1-i. j

1

., + t t l' 1 j Fig. 57 Melted Zr lead wire at 158 mm in D10. Phases include j Ni, Fe. and Cr back diff used from the locally melted f Inconel sheath. 250X (280669) I l 3 a 1 i d i j. ? i ? I. i i 4 8 l l l 1 3 92 i ~

i l l 6 >, f*. g l

• $a i,

. j. 4.* g ;+.I. " g.4 3 N 2 $~ s g a. '.

&* y~

(. 4h.w a.4 y r,' \\ :,..x.;... - 1 Q* 5.,; ~. lf \\f y$ ~ ' [y,y, s H 4 's fWb . y r . 4 ' W g )$ @W8 k C.. i ' h, h,1 Ofly %w h6 + - o e:- ,em s. .:o ..g+ .( . +- m,(,..,,,,+, g., y, y.e;%y, j -~ -. 2 P i i l i a i J Fig. 58. Layer of debris on outer surface of D10 at the 82-mm elevation. 250X (281852) l d i 1 s 93

l 1 l i i -~ t l l i i a y .:. n v ';y A i 1 A, d -'s 3 % 4 ~$4 p". th Ykd ow ~. sq - ll;f&g.y '

• pyg c-g;.

.c..... ..i - . k $ ,..[t 9 a3- &~ 4 .e, 3 . v.n V; y r., y c a"

l r f{.

r < w}[7' ' f : .f_ .7 .;,.f, __ >r

• l;h' f Y_

'? gm;rX_ l, 5..{-.> ;.*; y. y%,4 4

n '$;'r; n;,@j

.+w 3.: ~ ghn : - 5 ?l A - ~, s, _,' ' ;y:,1,.

lp:na, s, ;>

-r. n M:ftQ !m?j M, re.6.; ?;Q.1' '.,3 n. hl $ r 9* ,x, 7, ~..g.a %p ':t ?a [q ~. & ?.; 17 1 y r.,,. ~ i'..* $2, 4 ^Ca-4 t + ip s. .q/;4 . [. +jg ' ? 4 ft fith;jy .g . y;, m.

• T

,g4L W.5 ct ~;. V

3.,.

<}, e ,,r =. i i k

]

g 4y4

y !q O p[;?

r 1 (- '=-;fy " ;y 3 q; 3a9 s - +-, v

ay;

^ dye, n'rs?fyrv *ven'lw~t vn t e L ^4

t' :

a l;;a h....... L..t...... I. e t.. :s :sh.. Fig. 59. Elevation view of nozzle segment Ell. (282579) 94

hk)$h;, 1 u .e e x.7 .p%

-. g 4

$? kD4 }('s at . wh:5 % .i f, ; i j y ' " QL, P ..m .N hyy,rc-pis l l

wedy xf

• n*meww

_ ::t 81'l8ll'l'll'j818 'l'l'lI'l'l'8 818l'll'l'll*l'll'l'll'j'Id i. 1.,5... i. 1. %.... t.,1.1,5..... l.....1<.......l.....17..i...l. 1 Top (stereo pair) t f l i i n 4 e h,I/ f 4 s / ./ WE&- g lk l- ' DM 2 4-g***** pgg 2. {l'l'l' '3 'l'[ t ' '. ' / I'l'i' l .l 3,W m i &,i i M $L Z A Bottom t Fig. 60. Top and bottom views of nozzle segment Ell. (282584) ? I l l 95 i

4 8 a .i 3 3 3 3 3 4 I 1 i 3 i 3 o 8 o g N M y W y g 4 ~ N U m ms. g -m A m m e i - " -T ' M h A w x x A x +

=

b hams %g'> $' l . h.gg *'. .s'.,' g _? 'o 4-v g e 6 ,s. o A I 3 I o 9 8 7 6 5 4 3 2 1 0 0 g i i e i ) - 01 E,o - 02 C - 03 S - 04

~~

- os r; 3,o - 06 P ,o - 07 a ? i - 00 n"c' - 09 ? - 001 - 011 - 021 i dehcnL( neltLsoP.sv stlvLteR 731 sC latoT - 03.1 _ a41 69

l r i 4

$i l

l 1 9 ;: 9 y j h^'y - i 4 I fi 4. e i o l i 4 1 l l l i l Fig. 62. As-cut transverse section at 274 mm and longitudinal section through top of Nozzle Ell. 2X (280522 and 280528) 1 s i i 97 1 ~

I i i i i 'k - IIs E.f ft i' - yp. 14;s g-a ~- I

e.,

g;,'.

4...

';..[, % 7 e W 's,['. %. W l 1 h ? '- _ -Q t.;, ; h ?.. . 45

• ~'t-i 4

w l- '..da f.,n ~ 9'. ' f: '.' %" .j, _ ^* j Fig. 63. Fuel debris in the top of Nozzle Ell-(Original at 25X. reduced to 9X 280636) l l r l 98 i \\

1 A y L,x 'i f

• ?

h. e -y'[ e-gl. ^ a. jj N'2 9-. t p >,.;a ; y w w. S i' L i.,4

j).e q;5'c i

i I ig,i ~9 - r-r. 4 5N-S l Fig. 64. " Micro-folds" with trapped fuel debris in the j outer surface at the top of Nozzle Ell. 1 g a l M@ ) s ] 4 i i c:* a s

=

- v' \\ i ,3Y, ... Ny,. ,g J r, c. m i 7.-. y'

m M

i 1 Fig. 65. SEM image of fuel debris attached to the inner i surface of Ell at the 274-mm elevation. 99 1

IQf jf hg;r. T uf Tg..j. ' t' r v (- 4 I s e L l 4. -s

e y,;

l 4 'r 1 l ? I Fig. 66. SEM image of surface reaction at 274 mm on Ell. Ag-Cd nodules are l evident within the nozzle material. f i .~ ? s 1 r l Fig. 67. As-cut transverse section through Ell at 220 mm. Small gray mass at 3 o' clock may contain f uel. 2X (280525) r i t 100 i I i

l l ..l ,,..w.. 4.' (bh!Yh, l4l $ $,4.S.k.,g$ [Q g:.,_.,,;_.., . 7,.. :3

.;,;, '.

...g

,m y;%,. i I Fig. 68. Flaking surface debris-bearing scale and surface-adherent scale beneath it at 90-mm elevation on Nozzle Ell. 150X (281913) l r a t .e fk a 4;d i i i,. i ?

• i

~ .r. I t 4 t f ,-4 ./ i 1 .V l j f Fig. 69. SEM-BSE image of scales shown in Fig. 68. White dots along 10-p inner scale are Ag-Cd particles, i i i 101 ~

s t i t t i l' t } i e i i 6 l IX. APPENDIX 3 I h This section includes the descriptive data j sheet for each specimen examined by metal-i lography. SEM-EDX, or hardness measurements. l lll i i i ? I ,1 ) s t t i l 1 l 1 I i .I l i i 102 1

=. i Date of Sheet Preparation: //[92 OECD TMI-2 VesselInvestigation Project l Sample Examination / Test Summary Sheet Sample Log No.: A gfg/g/ Sample Source (check one): Vessel steel ,Y Nozzle Other (specify) i Guide tube Companion Performing Organization: Principal Investigator: Sample Core i Grid Location'- AAL - Adcr/z/ S L. A. /Vehrgesv-K j_ g l O Sample Location Description (attach diagram if necessary): Se /e is fro,,s 4Ae J: eve /ed A;p & JAe AD2 /e c W //2e. .2 6 3 mm e/evah*oit. Samyle i Covers O.D aerd E.D.5urfaces ist er feansve r.,e Vieu). i I Examination / Test

Purpose:

/. Defeneritse. n afure oA B"Y Surface cb y's'/r l on oz> aad .rb .s'urr' aced. t of nozzle maler/a l

2. khrmine ce Aear.Surfac$.

sthb~ i Examination / Test Technique and Formatt!ng: l pfg/a//pf y eed SEM-EC)X, A O fi'* / y:?Ac /eg y L.s, SEM /m9es, and W-ray Sy@ f Examination / Test Observation or Results: // arc / ness /3 /672 7 M. c.6 -j.o p //,th k /ayee em. cb and Zb wiK base m e /a f. i surfaceg, Afo in kt ac hk r co ~ e I one d %g e s t k o r, "/e.s i nors -uniArm in Layers-are / {e/ata.c ar/tc usi/4. cd A /ocaR~s >=e - ete L ie. A l. Tof b-me/o /.parf s d ofAer.s ricfr tr is.Z~ne. Geo, U-2r fue /.s/ weds. Eme 50,1 Cther Parent Breakoffs Sampi Log Nos.) and Purpose):d26ASAc3Ent, M AM $ 42f,42J/ l 426ASC. ) l Comments: l f i } Acd additicrial snects if r:ecessary A-1

i i l Date of Sheet Precaration: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g p f,4 3 / Sample Source (check one): Vessel steel t/ Nozzle Other (specify) ) Guide tube Companion Ferforming Organization: PrincipalInvestigator: Sample Core AWL-Mer/7M L 74 46/ wark [g " " Sample Location Description (attach diagram if necessary): S ai,p, /e is from. cen & of' noz2le a/ /Ae 283 mm elevak~ Co,n'abrs nisfrume,r / s/nug and' fuel messes. 1 I L Examination / Test

Purpose:

kferme nyQ of fue] clebris, insu/a for ma ferlef. 2n d Comf.SiliOM-of ins /rurned EdireS Y l*Corf7aSi/rk of c et-a.nte i i Examination / Test Techniq/syyhy e id see-sox. ue and Formatting: qa?;ca/ me/- f i Examination / Test Observation or Results: } See. refki h b,f./C I I Other Paren(Breakoffs (Sample Log Nos.) and

Purpose:

./24A/S/ (SEN and hardness), f,z{, 5,4 QEM sad ktrdtess -f26458 G4ard'nesaf l 4n Asc 63EM. Comments: r i f Acd accitional sheets d necessary [ 'l A-2

Date of sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: gggg Sample Source (check one): Vessel stee! /Nozz!e Other (specify) _ f Guide tube Companion Performing Organization: Principal Investigator: Sampie Core pQs1/4-AfC7"ffM A.4 WeAnB/*N f s Sample Location Description (attach diagram if necessary): 5amgsle is fro,n. oufer suc&ce of no22le l c1/ /%e 7 7 mar elevaz%, Examination / Test

Purpose:

1. p

/~gg Alez2le mictcSb~acN/~\\e.9 A* Cie {/-s, 2r,c/ /za&neSG, Examinationfiest Technique and Formatting: W' SEM-EDX,, onel Me/aA6 i A lopLs, SEM images ud W 90ecbg Opkcafp'baf a,d' hedn' ess me-saru en fs. Examination / Test Observation or Results: W micxs/n<cM, sek /e d,) 0 /2. //s dness is /69.t/ 5 1)PM, Are/u dr% measure-eds on 426A.S~B. Ao di'scevible.rarfxe lay'er t u is recoad n exWaNeu prod'uc/s psfes. sam e Cd'(~ h, Y (J-Zr-s /u e / pa eke /c, 33' % /40,u, wa.s farLee(cfed s*n s ue/2 cc, Cther Parent reakoffs (Sample Log Nos.) and

Purpose:

./26 AM/ $E# 3ad -f26A24/ C<EAO, f24A5BGfad""s).i 46A5dk A and'a es s Comments: Acd accitsonal s.eets if necessary A-3

.j Date of Sheet Preparation: OECD T&ff-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g ggfA g Sample Source (check one): Vessel steel VNozzle Other (specify) Guide tube Companion 6 Performing Organization: Principal Investigator: Sample Core A n t.- M C r,/. T P S L A AleAnark ff"~ Sample Location Description (attach diagram if necessary): S S.e /e is hm inner Surface

• E *
• 2 h" 2l

/be 77m,>, e/eva8en. i Examination / Test

Purpose:

-tVardness Examination / Test Technique and Formatting: DF// Examination / Test Observation or Results: l /69 2/5 kP//, NE/ud rnexuttmeh //atdneSS u]&S OL 426ASA, Other Paren(Breakoffs (Sample Log Qos.) and

Purpose:

1. 24A/8/[Sc/Jf 3"d bBN"'es%s 426A1A)/ G~EN),42MSA(nref SEAf,4petbres 4'26ASC(SGM Comments:

Add accitional sheets rf ne::essary A-4

Date of Sheet Preparation: OECD TAff-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: $9fff5C Sample Source (check one): Vessel steel Vkozzle Other (specify) Guide tube Companion i Performing Organization: Principal Investigator: Sample Core Am-mcr/rps 4 -,4. Mesn ark "2*g "; Sample Location Description (attach diagram if necessary): is -from cenAer of' nozzle a/ /Ae Say/e 77 mm eleva Ak, Ik/ade.s aoz2le ID <ned I/t S lr a m e n -f S h i Examination / Test

Purpose:

S~ / In G""u lRS h% >e s7afare. Of me/s/l$'c o.si/s, 9 me.spad me/24htgr*ca '73l"% o E.ZD Surf 3c.e cle & dirk of in.Sfrumexf c{ u)ites f Examination / Test Technique and Formatting-Afe/snn Y and.s at-spx. yieaYe$4 p /cgraphs,SEM htyes, Dad M Y'h. Examination / Test Observation or Resuits: SC e-fC >C b, f. //. Other Parent reakoffs (Sample L Nos.) and

Purpose:

/J64/8/ @N M i hardees 42642A/ ), 42d>ASA (ine/,5f/f, dadnessh 4.26As (?>ardness Comments: i Acd additiertal s.Seets rf necessary A5 )

5 i Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet l Sample Log No.: Q 4'2f 3/,4/4 / ozzle Other (specify) Sample Source (check one): Vessel steel N Guide tube Companion Performing Organization: Principal Investigator: Sample Core ga-ar-/.rtos L,,4, A ermarK

• }'I*";

{ / Sample Location Description (attach diagram if necessary): Sam is a fran.swese secfibr a+ /Ae 24/ ~~ p/e e/eva fr on a//de ouk'r-suefxe of Me gozz/e. Sa.,ry e cap /ures moHer itoatle maferie / l Brt d kaffel Surface clebri5 Examination / Test

Purpose:

DehermIne-n afure. e f enela//$'c aad ee M 12-A in He .sh-uc 1%re. H. ace / ness f ases Examination / Test Technique and Formatting: sEM -e.z:>y:, m e la//g ra,oLyl. k 4 OX fMlfa

• f oQ9 s,

$GJG{ M%eSj ka/ Examination / Test Observation or Results: Afe/s/ sse cag/af,s aumero u.c ydestcal bubbles /bbce is C - ep/e/ect Zr7conelh3M*-4.sfe-o.2 de),. Babble.s codain vyer-elepost/ed'..Wrudares M* / l'o n Yas*q /49, Caf, fn a d Af/ pod Se*,' Ca and 77 afra Sund, 'bindeo, o r ma frM

• f O' ~ '"I" L Cera r. orc pfage is a I

i.sfa. ds o f LJ-ze hpyypq es,y.,3ffe.,7sf;) 42 / ces fansg -ce" U. Had- ~ hn e Qyc Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

94 3/AZA (SEMh 96.B23/ (SE/d asc/ dardr>essb Comments: Acd adeitional sneets if necessary A-6

t Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examinatior(rest Summary Sheet j Sample Log No f3/AM Sample Source (check one): Vessel steel LAfozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core I Grid Location: i ,$NL.-Mc r/&PS L i4. Ale / mark y29 l Sample Location Description (attach diagram if necessary): /o r y/ / di/udinal seck Mroq4 /Ae Samp#/e is a 7b l mid lane. Samp e y o' aozzle a e p captures one.r.o sueface no=2/e a d coce foehioe o $ krSfrans ed clebeis is ce,, le r, and lexlh /ead. (See /~ij 8 hc Examination / Test

Purpose:

DB/ ermine r)a here o f rne faASc and Ceru/c phases. t Examinationfrest Technique and Formatting: Me/shpre an& SEM-EDX. .wx op ,oAoio a,s sex images a.s enx.sp,g. Examination / Test Observation or Results: See /ex8 p.7. i I Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

A/Al &EP/i;ted8ardneGs W 2 d> B 2 B ( m / M 4 & p Comments: i Add additional s'eets if t ecessary i r A7 ~ t

e Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No Nf[28/ Sample Source (check one): Vessel steel v1Tozzle Other (specify) Guide tube Companion Performing Organization: Principallnvestigator: Sample Core Gr o tion: Sample Location Description (acach diagram if necessary): W ansvers<~ Sec/rbn .2 7' ou:Aer-sueface af /be ~SS mm e '* v a b

• ors, Examination / Test

Purpose:

Y#'Y h /enn/se /1a/vec o$ S" f~ *W an d irozzle

hardness, Examination / Test Technique and Formatting:

SEM-Epx ad M badas, Examination / Test Observation or Results: //ar/ ness /s toz f 28.2}FN,l M r/r q s u c h c e hyeri o.s irop rich A Ce,fobnAf oXrde, Geeasi*oitaf cfepvs,A of 4/ (A" f O,y) r% /nyen e/gvanH4 .%me cen%/ ind' mar 4 era /s in bye r, su/ Me c grain boundy [ Base m a l a / i.s Inc. Seo. Occaerasa ( mp Son p . phases ir .Z~it ceire/, Ju r' baw% o /f

carbides, j

of /Ae base nefa/; frobably as/rdos se Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

W268/A/A (SE'M ae/ barAees 426 S/AZA ($f,ff} i Comments: Acd add.tional sr.eets :f ne:essary [ AB f

k Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No ffC/A/ Sample Source (check cne): _ Vessel steel _ Vfiozzle Other (specify) i Guide tube Companion l Performing Organization: Principallnvestigator: Sample Core 4ft(L-hfd;7~lf*;?$ L,,4$. A /8 h n 2 r 5 / Sample Location Description (attach ciagram if necessary): h Df SCCbbx l 70kgk MG it$$le. / cap uces 01:, zo as J Vy

• Surfas.

6 ExaminationfTest Purpose- 'I' N #A .T%/es'snine /7 2 lw-e Dl 'f A4e ba'e surfaces an d /A e ec,in?as/Au s /

mehl, r

Examination / Test Technique and Fermattlng: i SEM -fDX. SEM images and EDX -YMC}ra..DPH rn ea su re-e n f-s, Examination / Test Observation or Results: .Se e hexd, f. l5, Hei7>- base mela / &S mma I DPH was .Tnc. foCO.

1. 2/,, C/4 2 (m el),

Otner Parent Breakoffs ( ample Log Nos.) and Pu se: 42 C/A.38Gne 424 C2A (SEA 4'2 & C/A.3A((m et 426 C2Cl bar ness, 4.26 C2.D m e f. And SEM. Comments: i Add act tional s,eets if necessary 4 s A-9 l

P e Date of Sheet Preparation: t OECD TMI-2 Vesselinvestigation Project Sample Examination / Test Summary Sheet Sample Log No g2f C/A2, Sample Source (check one): Vessel steel

t. ffor.:le Other (specify)

Guide tube Companion Performing Organization: Principal Investigator: Sample Core A NL.-MCr/f/ 5 L - v4 Aleht>Bi-K C Sample Location Description (attach diagram if necessary): i .se:kost of ins /rumed s/cie Pseado fransverse fip a f stozz/e, ~s:8 mm elevalon. and debris af i Examination / Test

Purpose:

cri ;,,a//; fo de/ ermine no /ure o/ cerz~'c cle1:ws nex/ /c knA um en 4 s/"kg S G g ec<w n mniad ines,-m/ty an d no+ furMer-examined Seyssd 9x m ecec>olofo. Examinationfrest Technigdand Formatting: /Vld/a llog/-ap/c q}( rn B G r o f fe.S of $R)o fwd .ruefar es, Examination / Test Observation or Results: Sp,.aefu,e, de aMded'.,yoron s l w,,,,,,2[,,a/onun.: c.~< - w-q,, g y,_ /ga d Wshes OccSNW 0" reBCYe i r

1. 26 d/A/ (SEN M Avb ess)Breakoffs (Sample Lo Nos.) and Puedf26 6MEBC Ctner Parent se:

,, 426 42 6 4.% C2c/ Orard' ness. 426 C2z> (%e s'. m J \\ Comments: l Acd ac:htional sheets.1 ne:essary j A-10

1 + r Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet { Sample Log No.: j4 .fgg,g/g g Sample Source (check ene): Vessel steel vffo:zfe Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core 4yi,terf.r;os

1.,4. A/ ear > ark

• 'yy "

Sample Location Description (attach diagram if necessary): Lonpikdua/.seefiu of ces fra/ Asfru,ea slety Cap /ures ZD surfice a f fh e. ~ 90 rn m eleva-koa. so// diked akbris (7nasw/, S/rQe) ca r> d ine/aY/tc) ortco,cLif,/her side of ec~r eL//. Ins -rd er b4 $26 2nd Cen lathecd s933/rumenf / caws lE*/l 04 'b *b C0!9daib duri ff BrG /s'en. J Examination / Test

Purpose:

$rs jggf/ pk:> /clest di$ Cer7m/c "/773 & /al /k c /MShrnen l SbM'fg. anosafuS /u!cer rzo 2 2 e. B N l COW A0b #EfM O scever,- Santf e.freparaA22n. desi re d area. I Examination / Test Technique and Formatting: Me/afoysp/yt Op7'ica/' p24%hrey c L /o 250x, c Examination / Test Observation or Results: S&aefuees a>/Wa/n f maf dade/ies, enM l M Ae/ch a: d arems ol' oxidized wekd Am;/s<lh o/.s/raefuees fe, S4ese of 42fo C2A i es+ 4,,asbeds ore .s>/ tamed Zn:. too eso/ziy-l sagU,Zr; 11' aird ishnds af 74y Cd, (See. Fig. 37.) Other arent Breakoffs (Sample L Nos.) and

Purpose:

1. 26 C/4/ G3~4IN *dk/-

-f26 CrA2(dnee,s, -12/o cp n n;,s. a-c/ sestFN)' me/) 6 C/A33GneQ #26 C24 c3 i des 2c/ ase J26 Comments: 1 Acd additional sneets d :ecessary j A-11

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Ak 426C/ABB Sample Log No.: Sample Source (check one): Vessel steel VNozz!e Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core ANL.-Mcr/IPS 1.14. Aleirnar K Sampie Location Description (attach diagram if necessary): naar evere.see /,;,a fr - Me as fer o A nezzle af /he r64mm olevar%. C /ured stozz.le inner surface. wi/4.so//dfi inefal ogainsf it, and a,t oaw piece oe /Ae o,1 dua. Examination / Test

Purpose:

na-,4wal A // h, examise c era-<re OnyiiraU e Aueen ite>zz/e an d in sfrumex 4.s/nky annw%.s b sompfe. maa led fraorsm/seY, isof / lowever, fin a///, /ongishe Examinaiion/ Test Technihe and Formatting: MefaH cay yOp wayfit>yofs L A 6 2 sex. Examination / Test Observatior. or Results: S/rac/uag icfe,, //cg / .4 /Asse ir 426 c24; floSSiNy mbrS9 surfaces. Affer*osfruclu'eS 8So .s%//ar

/c, fAsse-it. 426 C/A3A.

Other) Parent Breakoffs (GriefSampiqLog Nos.) and

Purpose:

426 C2C / C/rardnes)s,f,2f>C/,434 (m et, t anct SEM /18s6 > 426C)/ 2 424 C2A 426 CRP Gne Comments: Acd additional s 4ets.f recessary A 12

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: / fff @/ Sample Source (check one): Vessel steel vffozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core kAll" W 7"lIPS L,A. We/>77 W E ff~ Sample Location Description (attach diagram if necessary): -r~rass m e sea-A o n fro,,, +Ae ce,, -kr o f itoz z le af /Ae 44 mn, elevalion, Capr%ced arfin f ins lrumen f.Slri , mefa ///c clebn'.s ' /r'di$'k in "" Rlws, and no2zle ahner-surface, (See-Fig. 36 tr +af.) Examination / Test Purpcse: bris h/enerare /?Blure. BS 171e fa f/l*c ir wie w,,natas. t Examination / Test Technique and Formatting: 4 Me/a//g' r7 y an d.SEM-619C O 4en7pho6 eapls 6 25a<; 3EM /*'%'s] p enxsm Examination / Test Observation or Results: SC2 lC-Xb /5-/b a r Other Parent Breakoffs Log Ncs.) and

Purpose:

1. 24 C/A/[SEM Nd 43M-Aess),426C /A2 ((Samp 4z 6 C/ASAGned,424 C/ASB(met) i m

424 C2C/(hardne., 426 C2D Gne/ pad SEN1) Ccmments: Acd adeticnal sheets rf ne:essary A 1'1

~. _.t i Date of Sheet Preparation: l CECG TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g gff {g / l Sample Source (check one): Vessel steel dozz!e Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core bz,ycr/TM L,4. Alei/rrarK "*yy*'i " j Sample Location Description (attach diagram if necessary): l - f r~ a,, g r g<- gf,b,7 of ou fee flozzle 5Ur-fGCG cW /4 e. 64 rnn1 e /eVa/rb>g. S B y lC CE;0NfC' I"' N v/2mm of surface a< cf exfen c(.s " 20 " "' I KD 22fe. I b Examinationfrest

Purpose:

$2rc(ness of 40ZZle. I l i Examination /TestTechnique end Formatting: i ON

• f.

.1VAI trieasuremen fs j 8 6X y i t Examination / Test Observation or Results: /3321 &, 4 ef 6 'rn e asu re m en f s to a s i ver e r Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

-/2/>d44/N)N I 426 C/A2 6e,d), 426 C/.4.54G re 0,)426 C24 CSEM.,, 42 6 C/d3B i Gne&, 42.6 C2.D (m~e/ pad.Scn { Comments: e t Add ace'tional snects if.ecessary 1 A 14 )

I Date of Sheet Preparation: j OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet ,46 42(;C2.D / Sampie Log tio.: Sample Source (check one): Vessei steel vNozzle Other (specify) Guide tube Companion Performing Organization: Principal investigator: Sample Core i ANL -Mcr/rp.s L. 4. Ale'her/C Sample Location Description (attach diagram if necessary): W3dVeMC Sec/rbn o f.5 ego en/ e / ou fer nozzle Sur~S@Ce af h4e 6 -f m m eleva f, on, Su rface. area is one l of severe.oblafien. I Examination / Test

Purpose:

2>efermin e n a luic of.":a/eriaI ** 'tozz /e surhee aard /c e/uc;d,Ae inecJran ism o f sueface a Ha t, e i Examination / Test Technique and Formatting: /We/a//ejra y SEk/ -Er>x analds-f f* car f/cgrySS fo SCC X, SEA l IMB% G^$ EDX pe/ra, l (See g /fo of/eM.) Examination / Test Observation or Flesults: he in e/r / bas staintsa / c o o,7 sihk o/ he. f;ec. Er. ed' A/C,0rbreifal ceasfi/u en f-s of. surface l's y er /Ad 6mp /* #Archescj fe, cr a d' il freseid Vbrics so o fo in siy: fica. +/y smaffen n o u., f s, 2 e cs., 4 .f ist Aryer 4 b 2e in fo hk Zn rher,qrun ufar-Wh ** fw,c,=eJrxf.%and C d' n24-n g(, (~f/2 -a, % 2,, in '2r-- A// surface b.,/ Mi e a//o As-cd o Other Pare $t Breakoffs Sampic Log fJos.) and

Purpose:

Ma d/4/M/* *f "d f2G Cf42 Conet'), }. 26 C/,4 Get.,), 424 CMJ;6(fwet.), #26 C24(SSAff 1 42c, cz ci (her dness comments: i Acc ac::ittenal snects d necessarf A-15

i i Cate of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet l Sample Log No.; A efy/Af Sample Source (check one): Vessel steel Mozzle Other (specify) Guide tube Companion i Performing Organization: Principal Investigator: Sample Core 4at-serf.7ps 4, A. Ne' anacK "*'y"; Sample Location Description (attach diagram if necessary): + l.ey//udina/ Sec/;e,, iArvuj} d. Bydermfe *'W"'

• i khe

~/35 m m elevafrq be/ouj durfx;e. %med is from

• rig k+ " Si de of riozz.fe.

an & inc /u des i oufer suefece., 6"ree of Azur.:,1pechr eas acrocs of rto2:le, of mela/Oc ud ce m yodases. l y, Examination / Test Technique and Formatting: Me4# eo .v-d.SEJf-ED% Nia:ro,pc /o,9A 9 L

• /o 2W*

e 25x ad mice

• gray s ad eux p, i

ExaminationlTest Observation or Results: [See /ex/,g. /J.) Ce-feof znc. 4;eo. Mamereas t N/Clafic,9Aase /s erbea45/ly %Lhles' in.shuc fuee, Needle -//ke Ws'/elef sfru e.fures associofe/ geners// tal/Jr bu bbles,,.>rs -r/cl (o xile ?), i o'ap-t>s/A /.c&u e r4v-es, w of usLmL 3ub6res C,,u., 4;,, v m Cr -reel ma +ria (o,eide) con fu<>t e r a a tc. masa es W so4*d/Aed i s.d 2,--reek /a ? ases, fue/ ycAare.s b (J-rte e In-si u.. Other Parent Breakeffs ' Sample Log Nos.) and

Purpose:

d'263/82 (m e d,/ hd 426 Dl B3 (mef), 426 pt.B4 (m e / a d h are'new). A/ SEM ex am in ako n. Comments: j Ac:3 accitional s.eets if nettssarf A-16 i I l

i Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project l Sample Examination / Test Summary Sheet Sample Log No.: y$ltf4.26DfB2 Sample Source (check one): Vessel steel MJozzle Other (specify) i Guide tube Companion i Performing Organization: Principal Investigator: Sample Core ANL -/V/C7fff~S l *.A

• YOI"?B'~S l

Sample Location Description (attach diagram if necessary): 4 ope,afe myfra a/ Lonfikdha/.secA% /4 she ~/3s mm e eva &n, se/ow kp.rur/a' ce. Seg,,.,ea is fe, He 'feff

• a f een /erfine, nex/ 6 du2> tB4, lap
• / #7ez 2 /e.

LC}pe of sNur-yecAnesS I paress Examination / Test

Purpose:

3)e fun /,, e n a /w-e-of m e b /d*c a d ce m /c b f ases. Examination / Test Technique and Formatting: i Me/> ry45 asd srM-eDx. ya 6 a/.zw a.t mmyyts /c zscx, SEM ,n m e s a-a FD>< pira. eas en /, a# ))O,/3.) 'erleled [See /ex/, Examinationfiest Observation or Results: %bbleb..&-a i /efath f(bu / V aae i.s C e r ~ 'c 'c .Drc. 6,co usi m J C,-eies chx,'de) win ;&c~imfed b!As o/ Zr- _g/,-d fied A e / p4 ases ou d y ac k fes 24 cdMy gn, h Other Parent Breakoffs (Sample LoqNos.) and

Purpose:

g2.4 2>/B -126 DlB3 (me+ v.Sem), -92a,.z)/3*f Gn e /,.sen v haebes Comments: Acd addinonal sneets :f ne:essary A-17

I Date of Sheet Preparation: OECD TMI-2 Vesselinvestigation Project Sample Examination / Test Summary Sheet Ah 4'26 Dl83 l Sample Log No.: Sample Source (check one): Vessel steel dozz!e Other (specify) Guide tube Companion j Performing Organization: Principal investigator: Sample Core m -n ergr'/ss i..g. m a

• 'py "

Sample Location Description (attach diagram if necessary): al g' he ~/35 mrn e/evafibn, Ee/bu>pinyinye nAy/zre Lon ifudinaf Sec6bry f /ir v u g. f t f/se Ap Surface. 59 <n en-f is k /de rig 4 + " of cen/ei-Abe, ned*f to 42b Dl.B/. On e o/ Asu- -yeo>new.s /cp actoss siezz/e. Examination / Test

Purpose:

yW,,y ,,gfsm of rnekASc a s d C & /c. fases. i Examination / Test Technique and Format +Jng: M e fa fog r a p/ ;Z s x a d ertbrog 4 c.ed SEM-CDX, i ls lo M X-placroffa e sEM ana;ps and ED.x p+a. fe_x /g,/S) 4W ",, Examinationfrest Observation or Results: (See l A'eh//<a w/Ssses o m esse.wtrq cr-dep Sco, some Gus bubb/es a-et u m e4 4. Ct--ric4 " /8/elels hefergeneous fomera fe i Bl>Sen i. "Cerwic" area is a ~ o A Cr-ncA m a.+rix can tainiq ace g o f (J-ree , za -rec u, e aa ri-c<a p/u..ses cn...,< c g ca,.aci,),y yae/ So//de*A'ed' ist-s/ i Cther Parent Breakoffs (Sample Log Nos.) and

Purpose:

-t.t AP/,S/6 e/ saa/SEWd 426 D/B 2 (%eh SEM), 416 2> tB4cket sf>f hardaess). Comments: Acd adcitional sneets tf ne:essar/ A-18

f Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet l l Sample Log No.: g g,26p/8 Sample Source (check one): Vessel steel VNozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core AML-Mc,r/It.S L -74. Alenrrark

• j "

l 0 Sample Location Description (attach diagram if necessary): //ucbh3l SSC.//on lb/~Cugk a g oxiN le,ei f / axe _ l /0nj/A al e -stJ5 mm elevanyn, he/sw Q.surkee. zw "/en s,s y nozz/e and' Seymes is s-, CnfantS eufer.Sur0&e. l [ Examination / Test

Purpose:

n gfu,c. eS r n e / ar / d 'c 3.*d C~ M 'k Agges gad Aar-dn' ess of' A4e 74rm er. Examination / Test Technique and Formatting: " A #' Afefo/4prafy SEM-EDX, D<d 'I>f# " at.zsex. Macy4,fo af.isxpieropfes Examinationfrest Observation or Resuits: [See hav#, / /J.) /aSf2 M Mefe9tc fase so@W;Aed" fm one// wiH numereas Cr~- exicle .su e faces. Hum aro-s pe,,.,7

• bairs Aavig Cr ~ric 4 n eea'le s la lele/s.,.Sorn e as den SN s * '"*I*

ener, tl devoid %1,.ble

• Rd w/fA Af 2r ggg&g Cr, Lake C, ~ b s d d'/ 4 omfer sudace is R

i,,c4s,L <7-;, "ceru,c.,c. ce, s. c-cic4 a 2-wa ni a, e

• o cerwe

1. 2 6.D/.B/d se / F SMA Other Parent B mef (Sa$$le Log Nos. Jid Puhse:e t v S&W),

akoffs S > 42 6 133 42 61>tB2 l' Comments: l Add adcitronal sr.eets :f ne:essary A-19

s t Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: gyg32B Sample Source (check one): Vessel steel 1-ffozz!e Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core g,yL-pfC7,-/~93 /.sA. hl8/n98/-K

• 'yy n; ff Sample Location Description (attach diagram if necessary):

Spmq jS /ou.sesf p/6r.e of Candhq on no22le wfer sudace. af Ae ~' 7 ~ ~ e I'va 'I'b ". P Examination / Test

Purpose:

pe fes,,,,9 e na fu, e o/ fAe C9^ Y j * ** 4l- [) jtXfttd/ /$ l1^ M *? S G-Examination / Test Technique and Formatting: Mela//p rap -y, SE74-EDX, 4 /= '00*x-MactmAofo d asx, micropto/ss 55&f 'im ag,es, EDX yfra, Examination / Test Observation or Results: h*s V 7'* " s ''"'c

• Rece is, ireegnlae/y '.chaped a 'd 14 furfaces. 2i;pse. mefa/ is iryy'Cr, clefwsiAs o,,

so % Ali, 72 g Fe Ge. 77 nq SS) Mn fo~**d as s ish.,a=. Nac&,ess is 142 u-

u. No Are9 ~

~(*=5 Fe -st A/I. of heavy " oxide

• wa n 2 s Ce ~

mefa/,One area Afa affegrapAy 3Lous5 firse/y d*sfersed, trito'c?ers/iNed;,,'"'bh'ESt5 l V w / Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

hlon e 426 b2 o or Comn;.'nts: Add add.tior.al sheets if necessarf A-20

e 4 Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: Aj[j f26.Z>$A Samplo Source (check one). Vessel steel VUozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core gyg,ygr/fp3 L. Af -/V8&?arE

• "hy "

Sample Location Description (attach diagram if necessary): eleva hk ol' 4e 7r~ an sverse .secf, bit. a/ Me-om, cenfer of nozzle, cgykres mas /- of Msfrumed Sfri of noz a fe_ inner-.Sueface, /9'8e tr7e/q, segm en i-clebeig ingo/ in annu /us, ad so ~ e arfic-aMc ala fe debris be/ ween irgro/ amd irozzle.4 Examination / Test

Purpose:

/ /de bb## 'E in hfer>,,he e n afure. a f rn e fau M *c fA e m e /*/h* . shards $,He k **"~ " f thgl^annu fu.s,He mefe/Ac'O,ca/ s/p/e af /he insfru,enf-c 5 '}) a** d u) ires, Examination / Test Technique and Formatting: a,a d.S&eV-E.DX, Afefahy'd lya / 2sX, irricsvf ra G/a.s '/c 2 sox. A//& crop e pfra. a~ d W SEM irnages Examination / Test Observation or Results: Ingof ampsdiam is ha bli-W&e-14 7Ae debers in Me k ul" S Cr-ricL far/id*les u.' i / U-Zr iqurih'es. nsih

• of.sAaeds (c.,ha/ar-) Je / ween co rA e i,., /eu - e. +

/eds are Enc. Goo + Mq,,

,,, 6.

e., / /eads are Ae <<=- & ~i r c,-aeus, wh/e eners radiah; ffos c< + nel suf4cie,< //y d 2,,;/tve of micros ue ke, Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

424.D 38/ (me[V 426D3C / Gnef, Sept ad Aa'=G<ess) Comments: Add ada.ttonal sneets tf necessary A-21

Date of Sheet Preparation: i OECD TMI-2 Vesselinvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: A gyg,33,8/ Sample Source (check one): Vessel steel Mzzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core Am.-uer/rps s.,4. A /e b n w ~ k

• 'yy" ";

Sample Location Description (attach diagram if necessary): T/~Bnsvers e seckc>t M /As ou&.scerfece eC de elev/a f*m, Cay ;wes ch h fl0Z2/e D-l fAe O m ar \\ B n/fmm se eos f of +4e surface, i P Examination / Test

Purpose:

EXans/a c flue raist 3 /ruc lterc

• b bSe 2* d defermr>re //s dardness.

Examination / Test Technique and Formatting: .uird ~2>f// measureire sa fs'. Nefafograpody Lelos /a/ y,x Gore /eled' w d e fc led),micropLoin Mac af wx..DPH measurem4s. Examination / Test Observation or Results: h WBl$"tenfo 0'E A MictcSfrae,fseec, /da:l c f3'SSeS e cas/.sfrae fzare evidenf. //a-dorecs is mi13.1>PH, Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

4% D.34 (me / ~d SEML 42 s.2> 3C/ Gere& SEs(, 4a"4'e's) t Comments: Acd additional sneets rf necessary A 22 'i

-l 4 t Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project r Sample Examinationfrest Summary Sheet Sample Log No.: A fff)3C/ Sample Source (check one): Vessel stael VNozzle Other (specify) Guide tube Companion i Performing Organization: PrincipalInvestigator: Sample Core i Aiva-Mcr,/. ras A.,4 Ale / mark y "; Sample Location Description (attach diagram if necessary): Transverse .seeftm from /he su fee.sueface of fhe noz2 /e a/ Ne 25 mm eleva ker. Cay /ures n25 m m of. surface an d ~. /o m,,, of dep/4 inward, Examination / Test

Purpose:

d asi/s Me Inc. 6 oo Eva/usle p., suefaee p exam,se graiot S&ac ec, an d cle f e r m a,x e Me bac hess i i Examination / Test Technique and Formatting-L SEM-E.DX,, c;ted 3>N/ mePS"* '"h. I J/'t.faWopraf Akekrof olo u,e fcled) DS 2.6 kj n'IC' f r3f 5 hlC b' 4

1. b

/oo and /S~OX) ltatclness measurco &.s iu. NY, Examination / Test Observation or Results: /99'f P'3PN (avg. o#.5 mess.) Alon-e<= a;A*brfum graik.sfru.c /1<re o S y"** 3xed f FD $bdi" S h s, S m,,.,' diame fer. Sme kne=4*xg up rr t d seen d phoses prese +. qsaru + yrecy;fa -//o ~bedad's 0~B d. wi F4isu g re;,,s an d a+ grain surfac.e fu i/ o/ /**r> e core de k.s o xl.fe, Ox/heer. m y ureib he fe~basecf(Eof ana/h S of L - /bic t a wiofe 5 .Por kcles alep ppear.s Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

42@34 (me/ t SEMf 426.D3.B/(me f %8 eras'ess) ~ ~ Comments: 1 Add adc.tional sheets d ne :essary i A 23

%/,b 2 o t. or sh..i er.o.r. tion: / OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No. $g/g/ Sample Source (check one): Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: Principalinvesti ator: Sample Core h)/-${$7l"ff l k Y d 2fg Grid Location-6// Sample Location Description (attach diagram if necessary): g". / 9,;g;h< din a / Sec.4b., NrD"[} b n h sf Go*2 2 le C a f 0 e..s 6 me fattic. .Shan s and he/ fr-a g n, e., f.:. i,z. o Stae coe. 1;cte c,.S 7erficu12+e m c /-> 9 and t?c= = /e-inn ec- .: uda c. e. Examination / Test

Purpose:

3e,ferm in f O 8 bu rC $ WNriS d;'nd -[* > e porficu /2 +e. ,rw t-ix. Examination / Test Technique and Formatting:

f. 7 fQ ),

$/8/p//ogrD A Bncl swr l~OY

• S G /1/

im an e= kd X ~ '*]

• f" '

g I ? Examinat!cn/ Test Observation or Results: verl Une (d/oo,yo)wgr\\N"lPa.- yes /,;/g f-jx is M fue/ sAaa-ds e vyy 3 co~po =,. s< w s c o-conpodIwn s > e 23 4! -H~/!2r. Sme cad: zed i 2re voriou s i&. fe m:s & p le a k l gwe e d .c k nIe== con ' Co/sen c .,.s /;iu e., + o5 ma leiv.bes ide.s U wnd.2r. Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

s t 42(,g/5z Gnex Saxi a id /medreas) Comments: [ Add additional s.eets :f necessary [ t e A-24

f i Date of Sheet Preparation: /[v r OECD TMI-2 VesseiInvestigation Project l i Sample Examination / Test Summary Sheet Sample Log No. gg g/[p Sample Source (check one): Vessel steel dozzle Other (specify) f Guide tube Companion j Performing Organization: Principal Investigator: Sample Core k)t)l.,d/4Yl_Z~/S d'.A Yt?AW5 $ ll Sampie Location Description (attach diagram if necessary); t Lor Sec 4 *o0

v. nc= /e I'f ''""T

} kthc iduclina/ inner- + d oufer.carfaceS. 1 i [ Examination / Test

Purpose:

De r'er,n:<,e n a fure of /20zzle de9 adaAbn.. l e 'De ferira,,e haebe=s. Examination / Test Technique and Formatting: flgfpf/cpa ,. GEN l~EDX, tr7Ecron,3rdne'cc. f qp6*ce/ p w/cc, S'=~M "nsges, X-r} 'P rR., &nd MY v'& la6G. Examination / Test Observation or Results: 4/ major SarfaeE l' esc fan f-0"N" '""f* c/sse 6 oc s/ soCe/e fe-fA're /"'*G 0"& %ic. o - fo/d ' **l '#~'fFW c.

u,.ja e

.sk ed ma Her fBr^c . u u a '~ p, +&ie s :.

c wgc c

ns.- i1 2a e=.:2mu lan. J 7 nea <~+ & Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

4.24,2,4 / (%ed anci SEM i Comments: ? Add adddicnal sheets.1 ne:essary A-25 r

i Cate of Sheet Preparation: j OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.:g g/ gf gg/ j Sample Source (check one): Vessel steel WJozzle Other (specify) _ Guide tube Companion l Performing Organization: Principal Investigator: Sample Core Grid Location: ANI-AAC,r/.Z~fS A. A. McMarg g;/ Sampie Location Description (attach diagram if necessary):

• 1r" ansve.tse Secf* n af nozzfe irirrer 5ur/*oce Seg men f-e af Me 274 mm e/emakoor. Cyfum me/a/#c i

/ an dewn on istn er-Surfa' ce and some parkculaf,e l ceramte clebris along in n er-s urfa' ce. Examination / Test

Purpose:

t pe l erm,<r e n a r%-e o f a,, e /ade e-ar><4e n .u., d -lh e c e r ami c. yc e/, c/es. Defermbre nozzle h arc /ne s s, t Examination / Test Technique and Formatting: Afefa //*gemp>9 aa d SEM~EDX) DfW measuoeds, l Macrep.fe,.a f g.6x; SEM images ud EDx pfra. l t Examination / Test Observation or Results: N fa///c runcleuse, cer,fijao gs soi/k. base nuefal ad' ce.,erudd 4 l Znc. 6eo ('arrayf is 90erl'rms).bulneldocwnenf&Cerewic c{al;ris a i he a 54ard's, fu e.f p a r-

,,. en fe-6x;/c) i e> u rei of fuet pip /rix (yield %;w agg omerafe Starg}tretes t

o,g exp,,na,ug mb core m i/eriaf ensfifu e, f=, e.g. ca, sr.,,%e /

• W "*ye-oA U/2, e,+ra, fco-e.oz -fa 2. z..%>e e. /~ / rd c*~s Mu~ 6 /*t i

Z*c s u'-f2'c l, E241) po/g matet,c, At sad n <;t/37.t4 DPJ/ t'.:t ys. el 9 erressurends reoc W areas o~ s unf i dar-dn e n 1:3 i i y Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

42d> E2,4(SE/t/ a;wa' Jrere/ ness) Comments: Acd additional sheets af necessary A 26

3 i l Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet A M.4 g g g f Sample Log No.: Sample Source (check one): Vessel steel VNozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core ,4a. -Me r /Z/;'5 L.,4. A/eimark E// Sample Location Description (attach diagram if necessary): TrBrysverse_ Sec f*n,, op ryo2z/e o u fer Surface Segme<+ af f4 e 274' m m e /evokous. Cafures ^20mm ofouke sur f ace, ExaminatiorFest

Purpose:

Surface it? lCracr4 bas ~l)e lerm/n c na/ure of any or-ct'epost t's, 58 Vermine r20 z z.le /?2rd'ne_gc, Examination / Test Technique and Formatting: A asal.$TE/Vf-E.DX,' yf// measueees enfs, Me/wS r Macrop,k>daa/ s sx; sm /,,,,,as o d aux spec fra. Examination / Test Observation or Results: (See /ex/, g..z /.) s h /// ens l sue /irce bfs// /o -2op dhic4", f.,/o b S /afers d>nd' /afen!, &cw s'ai,t Ce 9 77 % /Ae Inconef. F e,- r ic Lprincya//y / var'en Ynner-a/d u)//4,4/ 2,. pad'Q-Q C'e ler layars an con s'ain e d C4Zn, A, A/, Zr, Si in ad'd'//foss ffesc-fe d r egico\\ g lo !o en/r ancec/ Fe an d' Cr. Reac./fon M/eryranular 1572E,5X9' llV WrP$"Nn' (*aW*$'s EEa.sheeme%* wi/4 E24/. u Cther Parent Breakoffs (Sample Log Nos.) and Pu ose: 4' f EZA/ (WM asis' A8&1ess 2 Comments: L Add add;tional sheets if ne:essar/ A-27

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Ajg/ 5ff 6 p3/ f sample Log No.: Sample Source (check one): Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core 4x&i+1cr/IPs 4-4 /Vehr>Brk

• [*'*)' "

Sample Location Description (attach diagram if necessary): n~BMSverse Sm/for of itoa2le eufee surface af of swface the 9omm elevafran, Capfures a /S mm anc{ n/omm inl0 stoaz.le,* abg /S M my Examination / Test

Purpose:

'Dc/ art >e /s e nahre oA w .surfa c.e d'eps//s. b 2+ldeSS, Defermtorc. sg ozz /e Examination / Test Technique and Formatting: mm urm er f.s, Ay, SEA 4-EDX, }At/ /Welesfo e a arm.yec.ffos 9/ /So auf SW, ff f.6 x;miera j%//gcrof c / /ra, seu i., mas Examination / Test Observation or Results: Nenad/rere,& o.tamm Mick SC'fc on surface. Ce~ n tain $ rads At On f e -r/ck. rrs a lr / x, f ut-r~i o$ far/feu /a fe Shards a re p ein e,y,7/, 0 2,. Su a f, pop aa%e,e, p fy e, on st o22fe.

• fe _ kig ge d, / ~S p,fi e fes afap, tare fa)e, Ag b y fraec5.

are o,c z,n $3rd*'* ss is /9o& t 91>PN (avq. of 8 rnessare,-ed-s wdb E125) Cther Parent Breakoffs (Sample Log Nos.) and

Purpose:

426E4B.3 Gardness) Comments: Acd additional s*.eets tf r.ecessary A-28

e I Date of Sheet Preparation: OECD TMI-2 Vesselinvestigation Project Sample Examination / Test Summary Sheet Sampie Log No.: A[g,(26f~fE3 l Sample Source (check one): Vessel steel MJozzle Other (specify) Guide tube Companion Performing Organization: Principal investigator: Sample Core Grid Location: rAgW -/t46ffM L A W8/N W S f// \\ Sample Location Description (attach diagram if necessary): l Wansvers,e.Sec dbot of nozzle /ener-sur See al /de 90 mm efeveder. C duces v/.S~ min a f surface k d */S mm irtl0 nez2/e.j Dbuf.s -f2to E43/. i Examination / Test

Purpose:

Surface elef* Sit's. hlet*mine s?afuee oS 2nj De & mare /7o z z/e ka dness, Examination / Test Technique and Formatting: MelaA /-apy/ r.& x.h, SEnf-EDx, and 2>m hard' es n g sEm exam nof perroemed. Macsopc,to o l Examination / Test Observation or Results: &&eas /$ /ho 2/9WN (cW@. *f ? "'*#"**"S usif4 E4,,B/), Other Parent Breakoffs (Sample Log Nos.) and Pu cse: W,26s= stb / (Sa~/d cs" d " Am. i Comments: Add add.tional sneets :f ne:essary A-29

,m L i s Cate of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sampie Log No.: ykl& 4'ff[5,Q Sample Source (check one): Vessel steel vi9ozzle Other (specify) Guide tube Companion I Performing Organization: Principal Investigator: Sample Core >qa-acrfrps L.,4. A/ennart

• y ', "'"

Sample Location Descripticn (attach diagram if necessary): TransverG e Sec-fr'or of boWom Surkce (77 m m elevakon) of 7 emoved iris /~ men f 4 briot e Examinationfrest

Purpose:

Delermine nalare of exfranco"s m* fe'i' IS - t Examination / Test Technique and Formatting: y o e

e.,

i eX. Examinatior(rest Observation or Results: ///g/2nf//c..S/h;;prds' At&W6 CC/1lt9'r N N A h be ~

a n d,., s / c u.,, e n. 1 /e d s agearc>a some s urf*s beiHte feac /uees, bu+ roun da suges t duent,9 oc sG/ p iad' 4 L Ieyerahres.

Possibly ca.M9 debris rrom no22 e. ac9aisi k. Other Parent BIeakoffs (Sample Log Nos.) cnd

Purpose:

Yo/12. Comments: Add ad1tional s..eets if ne:essary A-30

e Date of Sheet Preparation: j OECD TMI-2 Vessellavestigation Project Sample Examination / Test Summary Sheet l Sample Log No.: A //f/~/f4If Sampie Source (check one): Vessel steel dozz!c Other (specify) Guide tube Companion t' Performing Organization: Principal Investigator: Sample Core Gr lo tion: g j, g,. ,,g Sample Location Description (attach diagrarn if necessary): Longik.dia,a / secfion of nozz/e inner-Surface "I'Y /Ae k (- 2 9 o m m eleva6&. Cyfures \\ a,( of /,,fer.s< uel' ace / hto 2 = te, in st'"" * ,$id'c - su p.a../>, u,<Lo~ + sm -- ~ ~ Examination / Test

Purpose:

bc,mA gafu, g af maferial ( l /IS'c r eo dam.; o/""' '", me a gfy7,, g

• a'e^ls.;

""~'c ,cozzAe exd Bi d /l3 N r C-Of gray, ll Kil~D ( "'I 2 5 2.. 1 Examination / Test Technique and Formatting: Sa$f-EDX. /V/e/e//cyrffa-d'a f 86x, m/qislos 8l250N* 5F f '. m e' Afgu o fc, M EDx sfec /ra. Examination / Test Observation or Results: 7 FAG /4G-esses /ia/y/ Inc.&oo hse ln annJu s is NeMe p:f dase s'.s 26..Znc. rf.K'-/ scc-12 P'. Aez2/e nex/ fa abo ve (cNa coadiai/ an Zn c. Cr-m " E' E*rc 'hersmic. is on .s'urfaces. sW-aad W-i-tel m's in Inc. nezzte. to -socy<-sta, fue/ (U-2r-).S/sorals fre,,ec{ ist r%A/s o/ So//c/a />e d me/, f is Ce@xta'e) en Ay afuzzle Gray 'tipu,-d' y/ lase a/ sfara /es-gy w&,g 4/ds en Cther Parent Breakoffs (Sample Log Nos.) and Purpo e: $2bflAW(Afe!$SEAf4arodeess Comments: Add additional sheets if necessar*f A-31

i 0816 Cf Sheet Preparation: h f2 - OECD TMI-2 Vessellavestigation Project . Sample Examination / Test Summary Sheet i Sample Log No.: f gg ggg Sample Source (check one): Vessel steel gNozz!e Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core ,4,44-Mc77'r cS A. A. Ale <:merK $,<*c""* y Sample Location Description (attach diagram if necessary): lCngiYtdina / Sc*cSen, /3 mir) ? ! 'Y0% ~2lC' Abu.h% h wd sid'c sae. faces, fSubsYhH_ybr.- 426 F/ A/.,\\ Examination / Test

Purpose:

D 6 erm in c. n a lu/~e ~d2n d' ex fen l Dl f .cuefa ce iderachort. Examinationfrest Technique and Formatting: $ /B //sj k CEM-8,X,st1/Cf E!btesS eu g6.&np6., x-ry spech a, Oph/a f Examination / Test Observation or Results: fueface oxida' % e! Ce asd' 'n:- we U-Z<- involvemen t,,4 / pene A ank behea/f 9X/de. a/easjN/g ale fW">< f A~9 d a' ""'/ N Wfa' e, y-le n:daIn wp(;%) = MokDP// w u. ~ A va. hardness Other Par 3nt Breakoffs (Sample Log Nos.) and

Purpose:

w Sc7/-EbX //20h Oh/- Comments: Add additional sheets d ne:essary A-32

Date of Sheet Preparation: J.f[C l2 / OECD TMI-2 VesselInvestigation Project Sample Examination / Test Sammary Sheet Sample Log No.: fffj y~/ c Sample Source (check one): Vessel steel XNozzle Other (specify) i Guide tube Companion Performing Organization: Principal Investigator: Sample Core Grid Location: kW&Nf$f )00 [ k d 8/ m 27t ,,$)/O ~ + Sample Location Description (attach diagram if necessary): af iso 22 /e s uchce frans verse .see fron af Ih e 24,6imi elevaken. Examination / Test

Purpose:

De ferm/n e r?Dfare 0$ S'urfDCe debrlC

• • d go:zz/e degra da6cn.

Examination / Test Technique and Formatting: /tfe faYcy ra $2Vf -EDX, &cI "'icrob5NlveCS, Opfies t ga ssy pk/cgrophs; N my "f**e - Examinationfrest Observation or Results: gyj-{pce plplakLse .2 m m Seeg l/~regtx.fB 'O sur-hee, 4 A/ pene ha ffen c + rr sun-ace c xicla +;o r Ob,e;rss,ie tais usi 14-Fe -oxide,,Cd-A 7 a " H c fe r. i ~% 4.- lay lers'. .u-2c/Ag - cd isn w e ~ 3yer. A ster ag e h a e d' # -S (S') Y!42n4I Fe-ricit / Cther Parent Breakoffs (Sample Log Nos.) and Purpose. YSAd 1 Comments: ?

• : $tional sheets.1 necessary A-33

i Date of Sheet Preparation: I/ 2-OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: gggg Sample Source (check one): Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core L.,i4 A e/ mark.

• $***f"

l i

4ML-Mer/.D65 Sample Location Description (attach diagram if necessary)

Sp,,, 'g is a h 2/1Sverse cross -Secbbn OS NL

515, en e,, f-

/rIn e a/~ lbC l$ "M1 0" 0% g Examination / Test

Purpose:

De fern,;,,e /Ae n a fure

• [

&nduIf redabo rilaferia / &At //urgj o e in%'de. co//epsed /uje, &d /Ae tr:e. l Zr-had

wirec, Examination / Test Technique and Formatting:

SEM-EDX, O fica /,pbo&grqs, Metafograp 3 and 4 f SGM isn9e s and X-r} pfra, i Examination / Test Observation or Results: . SYpin ler.:s .rfeef cat 4 ;/ da.S ex/d/'2efj so o A r/~~ reac/% fs 90 u A d. Ma fei-Ja / sh kde. Lc Cr - lefal have ha d' redox .Dcone I, Z~ uJit es genera fly 4an d, Grie. iuire a;fh Alz O, haula ko n; 2r- -Al eu lec.fic aff aredb melfed 2nd H,en t eaaked wifL Leonel hea fn 1 Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

/Jone Comments: Add add.tional snects if ne essary A 34

i J5/'91 cate of sheet Preparation: OECD Th11-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g[gA Sample Source (check one): Vessel steel MNozzle Other (specify) l Guide tube Companion f ? Performing Organization: Principal twestigator: _ Sample Core Grid Location: kNL-NCT/.r)R5 L '4< A eimsrK D /o l Sample Location Description (attach diagram if necessary): i 77~Anwerge Sec6% D-I-no22/c. :S urf='ce 2l lbe % W r&*' da r' /58m77 elevaf/on. Area is of gross 8 can %s ir flozzle. l l l .^ Examinationfrest

Purpose:

D ef ermin e nO f:g re ca d Co n r%>r f el CGvilics; ed micmc.few +sco o f no zzie, i Examinationfrest Technique and Formatting: pfe/B /l rql., C[hi-Gl>K, & cL rn Icro h afdn eSt., SEM />koIcyaf S

• x -ray Wm-A CyNea i

enes Examination / Test Observation or Results: Cas;/;e .A//ed u>ili fue/ debri= ir O rick 'n3Irh' I Inner Su rfaa.e s h a ve Cc-6xide) /syen A -Ccf g .cf,'s.3 e r: in, g ain b:an deries f ac = rn oll v<c nonle rnafrix. LargeanneA% +w.s s,9'a,rak (20 cla % in. nd l a a> t,2< Q .sha e of re. ins (i pA 3>P Indezfive of h le,L 4ecerah< re. l Cther Parent Breakotfs (Sample Log Nos.) and Purp e: ) g $fbf~Q fnfra/.Inc, nagd &#tI FA0hY '~Y# P " Comments: i Add additional snects if necessary A-35 J

1 l Date of Sheet Preparation: / h OECD TMI-2 Vesselinvestigation Project Sample Examination / Test Summary Sheet i Sample Log No.- gdf[g Sample Source (check one): Vessel steel dozzle Other (specify) i Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core Grid Location: kf/4-/Vf0t" k b k YS!MW p)O i Sample Location Description (attach diagram if necessary): . lY I 9 (e is fro m c ea, +es - cf U2=le d 'r elejkf;e,..,4rea .zAou>s rtezzl* D-

• d m* Nb C-ineg+ +rge.d t ~ a M-1 I

Examination / Test

Purpose:

gte, ge a3kee,8 /gof and l Seek e vi de,,c e_ C,;- e a a ser 4,- enaferia ( /o "-es o~ n ozz /e 2~b. t i Examination / Test Technique and Formatting: j /kefal/op~ryk, $c"i /-OX

• 0fCGlf

$7 S i j cem i.e, =ge= 2-s x-cy pc.+ra. i Examination / Test Observation or Results: y g ;3 G do /eQ/ U1CCn e I "'I ~" ,7 S "'l A I I y Sur(2ce. -Cel 11 dv (e s Ir I g3 re-rcci_ a re a c., orea u o A< c e S. Th- "4 nc22Ie de4c;e.J t- 'Cr$us id. 'cu> b *' gvkBc.e_ A*ct, ? rolo'u{a[q 0 :$E. & " 5 a s, e m*.-m* /em edh &Aer nu Cr* Ti M N. Cther Pare $t Breakoffs (Sample Log Nos.) and

Purpose:

42& F4A, 4x F~4C f Ccmments: i F Acd Additiertat s?.eets if necessary A-36

i i oste or sheet precuation: 9 ff2 - l OECD TMI-2 VesselInvestigation Project 7 Sample Examination / Test Summary Sheet Sample Log No.:/ pf/f fgC f Sample Source (check one): Vessel steel Mozzle Other (specify) Guide tube Companic n Performing Organization: Principal Investigator. Sample Core kAl!~W$YlffS b. k Y $ /72 W / Sampie Location Description (attach diagram if necessary): i 9,,, je

g

, o,,, surfbee & no2 We

l & *1 $ f signiRcc.d c/*bEr f' bc* O '"

• l

&res ahe w d oozzle. i Examination / Test

Purpose:

f f 'g b D g /e r n;;,r e /?B r%re O ! 5 ""# E'E

,, /e,.g ej;o, u);f L no zzle, w cl

/Aem.)al effech ir M e no zz le. \\ I' Examination / Test Technique and Formatting: //)8-l2llOrr-Bf5 ; $WA'l~ON. l J// f., gf k rn Qn ific&Nor b S~f0lE* icd,T. I i wegcap< s. Hy,5 ce&B-Land low irm weaG. 5 9 4E i* cps i 2md rea Examination / Test Obsery'ation of Results: M br*.= is & m o glare, *.( Cr pn d Pe o dde5 a k u) Sut I i m 2 i of Cr depleded I"onel "ey-l ?g,cke.le.s&a,g^rmsveseface

• hle.r2cicr itwo lJed Qr ox'A Q22(g M

pe e+ a +w. As-Ccl P&rkc lec '~d - c$ef elBCi CC%W S* f n 2,2( e 5,4 A Ciner Parent Breakoffs (Sample Log Ncs.) and

Purpose:

426 F4 A, A 2.6 F43 ; swe .P o rpose, Comments: l I t I Add acd.tional sneers rf re;essarf j A-37 )

-t f f i Date of Sheet Preparation: / o fl % i OECD TMI-2 VesselInvestigation Project t Sample Examination / Test Summary Sheet L Sample Log No.:g gfgggggg[ f / ozzle Other(specity) N i Sample Source (check one): Vessel steel Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core sk hl L - M c -rfM

j. 4, deiM wK y,*fcm Sample Location Description (attach diagram if necessary):

gg j= +k rh e rzc2zle s u r-fa e a .9 / ll2 9 2 rrk e le/a k o n. I; jgj'r

• crf ef;_

4, Examination / Test

Purpose:

3e femin e n2 h r-e ce Car-fsc.e. L Examinationfrest Technique and Formatting: /Vlefa//cgrs , SOl ~DX, p l'C&I fl*ff S, h S pecha, f84/ ren 3ges, Be d X-ra l Microh a ci., ecs Examinationfiest Observation or Results: NGQ rrwfrix conf =rds fu e / sba ds

• f V'

sfien s. I n. a g & d in f nc~ le. sur.4:e 'S'* *d a-

/0 C win /Ith* b]Sa lllb k & [~Y y lr. Ed(cX) /9]'2l'~a Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

. ?'.26 F58/; surIsee 'M + r'~'D * "'> '"' " "'

• Comments:

i Acd acc;tienal s. eets.1 necessary i A 38

i f Date of Sheet Preparation: OECD TMI-2 Vessellavestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g ggpg/ Sample Source (check one): Vessel steel Wozzle Other (specify) I Guide tube Companion f Performing Organization: Principal investigator: Sample Core i Grid Location: Ahi.-Mcr/rPS L. A. NeimarK Dio t Sample Location Description (attach diagram if necessary): ~ Wat1S verse. Ser/?b o f ou /cr n o z 2 fe. s ur-face t Bf /kC &C) 2l8Vahl:3rt- [Bf ttreS "/Smn / mm ch surface ared +7mm ist & tiozt/c, L i Examination / Test

Purpose:

h/erm/ne. nafure. of 2's S urface. l2 erS, Examinatior6est Technique and Formatting: 11//efa// rayd w d SEM-EDX. MN hareiness. /Wacn k a-b E'; 6X- ~S EN I"? V D~d O X ee 66 F.@ Examination / Test Observation or Results: "f5/M l 0 $ Vus,*3 ble lkicb:'oreSS, / /o / , lajer i l %a ' sh.some p aces; baads,fdi & fcoop-%, l p/en /s L,, d usere A4 Si, A, cf Zo a a' C ; g t_ eu/ar ba.ds a /sc, c, fata e d y 2,, Mo in A4ickes/ regn ol' hver. l Other Parent Breakoffs[ Sample Log Nos.) and

Purpose:

3 ll0ne_. f Comments: i Acd additJClial $ncets if Octe5Sary A-39}}