ML20070N306

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TMI-2 Instrument Nozzle Examinations at Argonne National Laboratory.February 1991 - June 1993
ML20070N306
Person / Time
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Issue date: 03/31/1994
From: Hins A, Neimark L, Purohit A, Shearer T
Argonne National Lab (ANL)
To:
Office of Nuclear Regulatory Research
References
CON-FIN-A-2220 ANL-94-5, NUREG-CR-6185, TMIV(93)AL01, NUDOCS 9405050325
Download: ML20070N306 (158)


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NUREG/CR-6185 ANLe-94/5 TMIV(93)AL01 TMI-2 Instrument Nozzle Examinations at Argonne National Laboratory I

February 1991 - June 1993 Prepared by L A. Neimark, T, L. Shearer, A. Purohit, A. G. Ilins Argonne National Laboratory Prepared for U.S. Nuclear Regulatory Commission PD ADO K 050 320 P

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AVAILABluTY NOTICE Availabikty of Reference Matenals Cited in NRC Pubhcations Most documents cited in NRC publications will be avaltable from one of the following sources:

1.

The NRC Public Document Room. 2120 L Street, NW., Lower Level. Washington, DC 20555-0001 2.

The Superintendent of Documents. U.S. Government Printing Office, Mail Stop SSOP, Washington, DC 20402-9328 3.

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l DISCLAIMER NOTICE This report was prepared as an account of work sponsored by an agency of the United States Govemment.

Neither the United States Government nor any agency thereof, or any of their employees, makes any warranty, expressed or implied, or assumes any legal liability of responsibility for any third party's use, or the results of such use, of any information, apparatus, product or process disclosed in this report, or represents that its use by such third party would not infnnge pnvately owned rights.

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NUREG/CR-6185 ANL-94/5 TMIV(93)AL01 TMI-2 Instrument Nozzle Examinations at Argonne National Laboratory February 1991 - June 1993 i

Manuscript Completed: February 1994 Date Published: March 1994 Prepared by L A. Neimark, T. L Shearer, A. Purohit, A. G. Ilins Argonne National Laboratory 9700 South Cass Avenue Argonne,IL 60439 Prepared for Division of Systems Research Office of Nuclear Regulatory Research U.S. Nuclear Regulatory Commission Washington, DC 20555-0001 NRC FIN A2220

Abstract i

l Six of the fourteen instrument tube nozzles extracted from the TMI-2 lower head were examined at Argonne National Laboratory to provide information on their metallurgical state, on interactions with core debris that made its way 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

lower head, the mechanisms, modes, and extent of nozzle degradation to evalu-ate the challenge to the lower head containment boundary, and contribute to 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 l

X-ray (SEM-EDX) analysis.

The results of the examinations indicate that some nozzles were melted off by interaction with molten core debris, whereas others were only thermally affected by contact with core debris, some of which attached itself to nozzle surfaces.

The elevations at which the nozzles were melted off suqqest that the liquid core debris was atop a crust of solidified material that apparently generally insulated the reactor vessel from the hottest debris.

The pattern of nozzle degradation was consistent with the location of a hot spot in the vessel at the E7-8/F7-8 location as determined by metallurgical examination of the vessel steel samples by others.

Based on the severe damage to some noz-zles and not to others in relatively close proximity, it can be concluded that the flow of material across the lower head was multi-directional and not uni-fled.

It is believed that a significant portion of the core debris moved across the lower head, from the east and southeast toward the hot spot, in a lava-li ke flow, the basal crust insulating the vessel and the lower portions of the nozzles.

The finding of significant quantities of control assembly ma-terials (Ag, Cd. In, Zr, Fe, and Cr without U) in the nozzle material and on nozzle surf aces indicates their presence on the lower head prior to the mas-sive relocation of core debris 226 minutes into the accident, iii

CcH1 tents I. INTRODUCTION...........

1 l

11. OBJECTIVES....

1 111. SCOPE....

3 IV. GENERAL PROCEDURES................................................

3 l

l V. EXAMINATION RESULTS..................

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A.

Nozzle M9 7

B.

Nozzle L6.......

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C.

Nozzle HS...

12 D.

Nozzle H8.

15 E.

Nozzle D10......

17 F.

Nozzle Ell.

22 VI. DISCUSSION..........

25 A.

Defining " Debris".

25 B.

Nature of Nozzle Damage.

26 C.

Postulated Fuel Relocation Scenario.....................

28 D.

Presence of Control Assembly Materials..

31 E.

Temperature Indicators 33 F.

Penetration of Materials into Nozzles.....................

35 VII. CONCLUSIONS...

37 Vill. REFERENCES...

101 IX.

APPENDIX........

A-1 y

Figures 1.

Grid map of TMI core showing locations of nozzles examined at ANL.,

43 2.

Typical in-core nozzle with seal and retaining weld...

44 3.

Lower head area and incore instrument guide tubes.......

45 4.

Elevation view of nozzle segment M9, as received...

46 5.

Top and bottom views of M9 nozzle segment, as received 47 6.

Gamma activity profile and sectioning scheme for Nozzle M9.

48 7.

Longitudinal sections through top of Nozzle M9 near the center (left) and at the center (right)...

49 8.

Longitudinal section through top of Nozzle M9.

50 9.

SEM-BSE image of multiphase fuel in Nozzle M9....

51 10.

As-cut transverse section at 241-mm elevation of M9. showing metallic and possibly ceramic debris between 5 and 8 o' clock in the annulus.

51 11.

Elevation view of nozzle segment L6......

52 12.

Top and bottom views of L6 nozzle segment............

53 13.

Gamma activity profile and sectioning scheme for Nozzle L6.........

54 14.

As-cut transverse section at 283-mm elevation of L6. showing a porous materis the annulus..

55 15.

Instrument string and fuel debris at 283-mm elevation of L6.

56 16.

Partially transformed fuel mass at 283-mm elevation of L6....

57 17.

As-cut transverse section at 77-mm elevation of L6...

57 18.

Partially transformed zirconium instrument lead at 77-mm elevation in L6..

58 19.

Etched microstructure of Inconel 600 nozzle at 77-mm elevation in L6.....

58 20.

Elevation view of nozzle segment HS.

59 21.

Top and bottom views of H5 nozzle segment.

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22.

As-polished bottom end of H5 segment, revealing only a solidified 1

metallic mass.

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23.

Gamma activity profile and sectioning scheme for Nozzle H5.........

62 a

24.

As-cut transverse section through H5 at the 114-mm elevation.......

63 4

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25.

As-cut longitudinal sectior, chrough top of H5 segment..............

-63

}

26.

Metallic and ceramic debris at top of Nozzle H5..................

64

]

27.

Microstructure of debris at top of HS. showing intimate mixture of U-rich phases (light). Zr-rich phases (medium). and Cr-rich matrix (darkest)...........

65 i

j 28.

Chromium-rich platelets precipitated in Cr-depleted Inconel........

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29.

Instrument string and solidified Inconel mass at the bottom of the H5 segment.....................................................

66 4

jl 30.

Shards of Inconel 600 (a) and fuel debris (b) within instrument string at bottom of H5...........................................

67 1

31.

Bottom weldment of the H5 nozzle...................................

68 j

32.

Top. elevation and bottom views of H8 nozzle segment..............

69 33.

Gamma activity profile and sectioning scheme for Nozzle H8.........

70 l

4 34.

1 As-cut longitudinal section through the top of H8..................

71 35.

As-cut transverse section at the 64-mm elevation in H8.............

72 4

j 36.

Metallographic section of instrument string and metallic debris 1

at the 64-mm elevation of H8...

73

{

37.

Eutectic structures containing Zr U. In Ni, Cr. and Fe at the 64-mm elevation in H8.............................................,

74 38.

Abl surface of H8 nozzle at the 64-mm elevation................

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39.

F" 3E image of Ag-Cd particle, and Zr-rich material penetrating-i suriace of H8 nozzle at 64-mm elevation............................

75 a

j 40.

Elevation views of 010 nozzle segment..............................

76 1

41.

Top and bottom views of the D10 nozzle segment.....................

77 4

42.

Gamma activity profile and sectioning. scheme for D10 nozzle segment 78 d

43.

Two sides of the longitudinal section through the top of the 010 nozz1e...................................................

79 1

44.

Typical area of fuel shards found at top of D10 nozzle.............

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45.

As-cut transverse section through 010 at the 266-mm elevation, showing metallic and ceramic debris inside.........................

80 46.

Surface deposits at 266 mm on Nozzle 010...........................

81 47.

As-cut transverse section through 010 at the 177-mm elevation.....,

81 48.

As-cut transverse section through D10 at the 158-mm elevation......

82 49.

Area of grain boundary separations in D10 at the 158-mm elevation..

83 i

50.

Examples of Ag-Cd deposits in D10 at the 158-mm elevation, showing Ag-Cd penetration as (a) stringers and (b) discrete particles.....,

84 l -

51.

Examples of particulate fuel debris trapped in grain boundary l

separations at 158 mm in D10.......................................

85 52.

Area of grain boundary sepaimtions in D10 at the 158-mm elevation, etched to show possible second.pbase and internal grain structure..

86 53.

Portion of thick exterior deposit on D10 at the 158-mm elevation...

87 54.

Examples of Ag-Cd in inconel at 158 mm in Nozzle D10..............

88 55.

Segregated U-rich (light) and Zr-rich (dark) phases in fuel particle in a deposit at 158 mm on 010.............................

89 56.

Instrument string at 158 mm in D10.................................

90 57.

Melted Zr lead wire at 158 mm in 010...............................

91 58.

Layer of debris on outer surface of D10 at the 82-mm elevation.....

92 59.

El eva ti on vi ew of nozzl e segment E11...............................

93 60.

Top and bottom views of nozzle segment E11....................

94 61.

Gamma activity profile and sectioning scheme for Nozzle E11........

95 62.

As-cut transverse section at 274 mm and longitudinal section through top of Nozzle E11..........................................

96 63.

Fuel debris in the top of Nozzle E11.................

97 64.

" Micro-folds" with trapped fuel debris in the outer surface at the top of Nozzle E11..............................................

98 65.

SEM image of fuel debris attached to the inner surface of Ell at the 274-mm elevation.........................................

98 66.

SEM image of surface reaction at 274 mm on E11.....................

99 67.

As-cut transverse section through E11 at 220 mm....................

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1 68.

Flaking surface debris-bearing scale and surface-adherent-scale beneath it at 90-mm elevation on Nozzle E11........................

100 69.

SEM-8SE image of scales shown in Fig.

68...........................

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Tables 1.

ANL Nozzle Segment Lengths Elevations, and fuel Penetration Depths 39 2.

Composition of Debris Areas / Particles Containing U-Zr.............

40 3.

Summary of Hardness Determinations.................................

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l Forevvord The contents of this report were developed 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 organizations are:

The Centre d'Etuces d'Energie Nucleaires of Belgium, The $3teilyturvakeskus of Finland,

)

The commissariat a l'Energie Atomique of France, The Gesellschaf t f 0r Reaktorsicherheit mbH of Germany, The Comitato Nazionale pcr la Ricerca e per lo Sviluppo Dell' l

Energia Nucleare e Delle Energie Alternative of Italy, l

The Japan Atomic Energy Research Institute, l

The Consejo de Seguridad Nuclear of Spain,

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The Statens K8rnkraftinspektion of Sweden, The Office Fed 6ral de l'Energie of Switzerland, AEA Technology of the United Kingdom and l

The United States Nuclear Regulatory Commission.

The primary objectives of the Nuclear Energy Agency (NEA) are to promote cooperation between its Member governments on the safety and regulatory aspects of nuclear development, and on assessing the future role of nuclear energy as a contributor to economic progress, j

l This is achieved by:

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-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 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 demand and supply for the dif ferent phases of the nuclear fuel cycle and the potential future contribution of nuclear power to overall energy demand:

-developing exchanges of scientific and technical information on nuclear energy, particularly through participation in common services:

-setting up international research and development programmes and undertakings jointly organized 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 the nuclear field.

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Acknowledgments The authors acknowledge the unstinting support and patience of A. Rubin, C. Serpan, and E. Hackett during the course of this work.

The endeavors of J. Sanecki for his consultations on analytical results: D. Pushis. W. Kettman, F. Pausche, D. Evans, and L. Essenmacher for photography, specimen prepara-tion, and metallography; and E. Hartig for manuscript preparation are grate-fully acknowledged.

The authors sincerely thank D. Diercks and T. Kassner for their consultations and being the sounding boards for many of the concepts documented here.

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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 1

United States Nuclear Regulatory Commission (NRC) and the Organisation for Economic Co-operation and Development (OECD).

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.

This report was prepared under the auspices of the OECD/NEA Three Mile Island Vessel Investigation Project.

)

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 instrument nozzle segments and two segments of instrument guide j

tubes were retrieved for metallurgical evaluation.

The purpose of this evalu-l ation was to provide-additional information on the thermal conditions on the lower head that would influence the margin-to-f ailure, and to provide insight into the progression of the accident scenario, specifically the movement of the molten fuel across the lower head.

II. Objectives The VIP has as its principal goal the determination of the margin-to-I 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 Engineerirg 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-i ure analysis.

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Thus, the overall objectives of the nozzle examination effort at Argonne National Laboratory (ANL) were to (1)

Provide information on the temporal and locational movement of fuel onto and across the lower head:

(2)

Estimate peak temperatures of the nozzles from their metallurgical end-state and (3)

Determine the mechanisms, modes, and extent of nozzle degradation to evaluate the imperilment of the lower-head containment bound-

ary, Data requirements provided in the Coordination Plan established the fol-lowing specific objectives for the nozzle examinations:

(1)

Determine the nature and extent (axial and radial) of fuel / debris ingress into a nozzle:

(2)

Determine the nature and degree of chemical and thermal interac-tion between fuel, debris, and nozzles; (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 (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, 1

2

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Ill. 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.

The scope of the examinations at ANL consisted of visual examination and macrophotography, axial gamma scanning (137Cs), sectioning followed by macro-photography of the as-cut surfaces, metallography with selected microphotogra-phy (some in the etched condition), microhardness measurements on selected samples, and scanning electron microscopy-energy dispersive X-ray (SEM-EDX) 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-ples were examined by SEM-EDX. the microhardness was measured on 21, and three I

were etched to observe the microstructure.

IV. General 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 surface at 120 intervals, of the bottom surface, as cut at TMI, and of the top surface, 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 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:

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(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:

1 (4)

Obvious locations of surf ace 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 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.

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 heating.

Longitudinal sections were 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.

I 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.

Microhardness was measured with a diamond pyramid indentor in a Leitz MM5-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

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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-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 j

l 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 /

temperature effect correlation, the effort to etch more samples was abandoned.

I V. Examination Results This section will describe the examination results on a nozzle-by-noztle basis, moving essentially from east to west along the lower head.

It is be-lieved that this was the direction of the principal fuel flow across the lower head some 226 minutes into the accident.

j The six nozzles examined at ANL were from core locations M9, L6, H5, H8, 010, and Ell; their locations on the reactor grid are shown in Fig. 1.

The i

damage to these nozzles provides a representative sample of the damage that occurred to all 14 nozzles that were removed from the vessel and, together with information from the eight nozzles being examined at INEL, provides good i

information from which to construct e 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.

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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-fled during the handling process before the nozzles arrived at ANL.

The basis for subsequently making the true identification of these nozzles was a compar-4 and the visual observations ison of the records generated by MPR Associates made when the nozzles arrived at ANL.

The mis-identified nozzles were H5 (nee D10), D10 (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 I

former identity, it must be recognized that these identities differ from i

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 observed 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.

For 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 ele-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 cut-off end to the particular elevation.

The changes have been made to better i

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.

6

s 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 concluded that the 137Cs activity was inside and not on the surface of the noz-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.

AL Nozzle M9 The M9 nozzle segment received at ANL was 254 mm long.

Based on a nomi-nal as-f abricated 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 candling.

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-zle: howesor, there appeared to be material in the central tube of the instru-ment strina.

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 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 surf aces through the top of the nozzle.

Melting of the noz-7

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 once-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 SEH-EDX system cannot analyze for oxygen).

What remains of the instrument leads (generally Zr wires in Al 023 insula-tion with Inconel 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, 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.

l 8

= _,

l 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 I

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 i

of enhanced Cr material, apparently Cr-oxide, was found on the surface, along with occasional deposits of A1, 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 i 5 diamond-point hardness (DPH), while the average of measure-ments from the bottom specimen was 202 1 28 DPH.

A summary of all hardness measurements on all nozzles is given in Table 3.

The low values from the top reflect the significant Cr depletion in this area, with the result that the matrix was no longer Inconel 600.

9

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 of f.

Debris inside the nozzle, external to the instrument string, can be seen in both the top and bottom views.

The 137Cs axial gamma scan, Fig. 13, indicates that the contained material is apparently fuel-bearing.

The nozzle was sectioned transversely at five locations as shown in Fig. 13.

These elevations were selected principally to attempt to determine the nature of the material that was creating the 137Cs activity inside the noz-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 arcas 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 A1.

The microstruc-ture of this particle, Fig. 16, shows that the fuel had been only partially translo med 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-l 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 appeared to have the darker grain boundary phase typical of the low-melting oxides of Fe, Cr, and Al.

10

There was a very thin, 0.6-1 p complex depcsition layer on the outer I

nozzle surface at the 283-mm elevation (top).

There appeared to be no inter-l 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 I

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.

There were no obvious fuel masses at the 77-mm elevation (Fig. 17), but l

a piece of metallic Al with Ti as a second phase was between the instrument string and the inside surface 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 UO2 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 oc phase occurring at the surf ace.

Other leads were also in vary-ing stages of transformation.

Assuming the material was initially a phase, the transformation to p would have occurred at 862 C if there was little oxy-gen present; the transformation temperature rises rapidly with increasing oxy-gen in the et 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 oxidize.

Because there was no redox re-action with the Al 0, the temperature was <1200*C.

23 L

l 11 l

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 T1 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 were damaged 6 is indicative that the material in the nozzle probably came down 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 i 7 DPH at the top and 169 t 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 the nozzle.

C.

Nozzle H5 The HS 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 the 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 1

l by SEM-EDX) is Type 304 stainless steel, possibly from the conduit that sur-rounds the instrument string, but also 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 i

1 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 isshown 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 V 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 is 1990 C.

In Fig. 27, note the porosity in the Cr-rich 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 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 A1 023 insulating material in the instrument leads.

The Ti apparently was 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 within 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.

f I

A metallographic specimen was made at the 25-mm elevation to examine any f

surf ace deposits, examine the Inconel microstructure, and to perform hardness measurements.

There was a 50- -thici. oxide on the surface, topped with fine I

13 f

I

i 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 stages of phase transformation, from - to a-phase Zr, similar to what was found in Nozzle L6 (see Fig. 18)

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 1 2 DPH in a region that was Cr-depleted.

The bottom sur-face, however, which was the weldment, measured an average of 217 i 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 i 8 DPH.

14

i l

D.

Nozzle H8 i

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 af ter the accident was broken of f 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 Fi T

at v pro 1 indicat s that fuel s 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 f airly well intact, but bent.

l Solidified fuel and metallic debris can be seen to the lef t of the string.

l The " goose-neck" bend of the ablated upper lef t 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 ?r.

Un~.ike the fuel in the tops of Nozzles M9 and H5, some of the fuel areas it, 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 combination 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

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 were found in the material higher in the 1

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 F

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 agglomerated particulate (<50

).

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 reacted with liquid Zr that also contained a large quantity of Ni and i

smaller quantities of U, Fe, and Cr (Zr:0 -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

J Zr from the Zircaloy guide tubes: and Fe-Ni-Cr from the stainless steel cladding.

Second, the Zr:U atomic ratio of the surface and sub-surface reac-tant, -8.5:1. is significantly different from that of the particulate fuel found in this nozzle and in the fuel debris in most other nozzles where the j

content of U is generally greater than that of Zr (see Table 2).

These two points strongly suggest that this nozzle was ',, contact with material from the control rod assemblies before the major fuel flow arrived on the vessel.

Microhardness measurements on the nozzle averaged 133 i 4 DPH at the 64-mm elevation and 148 i 7 DPH at 108 mm.

These values were among the lowest values measured on inconel that did not exhibit Cr-depletion and reflect a j

high nozzle temperature 64 mm from the vessel.

E.

Nozzle D10 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 l

-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 surf ace debris.)

Just above the 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

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 nozzle'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 particulate areas are given in Table 2.

The. significance here is the particulate and inhomogeneous nature 1

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 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 in the annulus but none on the exterior.

The exterior surface at this eleva-tion exhibited 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 products 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

7 i

almost pure Fe (oxide).

In some areas this layer contained fragments of a mixture of U-Zr and Ag-Cd.

On surface areas where there was no ablation, the surface layer was =1 p thick and contained Al, Zr, Ag, Cd, In, Ti, Cr, Fe, and Ni, but no fuel.

1 The transverse section at the 177-mm el< : tion, Fig. 47, shows an area of fuel debris on the exterior surface, 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 surf ace 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 surface 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 surf ace, 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 track 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 l

i 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 i

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-l crostructure of this area, Fig. 52, indicates a very large grain structure I

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 i 2 DPH, indicating that a very-high temperature was achieved.

The area was not depleted in Cr, however, as was the case in other i

low-hardness areas.

I 19 l

-.~- - -.- _ _ _ - _ _ _ _ _ _ _

Although a cast, dendritic microstructure was not brought out metallo-graphically, it is nat inconceivable that at least one side of the upper'part of this nozzle was essentially molten, or very close to it, the apparently 4

)

undisturbed exterior shape notwithstanding.

Measurements on the nozzle cross section in Fig. 48 indicate that not only is the center hole eccentric but the outer surface is as well.

The outer surface has moved outward by =3.5 mm op-posite the eccentricity of the 10.

The fact that the inner instrument tube is 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 side of the nozzle outward.

The large surface bubble at 177 mm is another in-dication of melting of at-least the surf ace.

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-trasted to the smooth surface of the ablated areas-on the surface of Nozzle H8.

The massive surface deposit diametrally opposite to the intergranular 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 Cr-depleted Inconel (white areas) and physical mixtures of oxides of Cr, Zr, U. Fe, and Ni (gray areas).

Part of the original nozzle surface is assumed to be the thin gray line of Cr and Ti (oxide) at 5 o' clock in the figure and ex-tending upward through the wide band of voids to 12 o' clock.

The gray phases to the right of this line are principally Cr, Al, and Ti rich, with some U and Zr.

The Inconel matrix to the right of these oxides contains inclusions of Ag-Cd. as does the large Cr-depleted Inconel masses between 6 and 8 o' clock.

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-lar-shaped particle at the outer edge of the deposit shown in Fig. 53.

The microstructure of this area, Fig. 55, shows segregation of the fuel into a U-rich phase (89 wt.% U-3 wt.% Zr-8 wt.% Fe) and a Zr-rich phase (25 wt.% U-57 wt.% Zr-18 wt.% Fe).

Such fuel concentrations were the exception. Generally, 20

i fuel constituents were more randomly dispersed in other phases of Cr and Fe oxides.

The areas containing the larger amounts of U and Zr were in the outer areas of the deposit.

Figure 56 shows the instrument string at the 158-mm elevation. The Type 304 stainless steel conduit was almost completely oxidized but the Inconel 600 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 instrument wires had reacted to varying degrees with Al 023 insulation, result-ing in oxidation of the Zr and reduction of the Al 0.

The relative free ener-23 gies of formation of these oxides suggest that a temperature of at least 1200 C was reached for this redox reaction to occur.

One instrument wire, at 5 o' clock in Fig. 56 and shown enlarged in Fig. 57, apparently had melted and j

sent six stringers outward toward the cladding..An analysis of one such stringer indicated only Zr, but, because the melting point of Zr is high at 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 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-cause the Zr-Ni eutectic occurs at 960 C.

In any event, the temperature of the instrument string at this elevation was at least 1200*C.

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 i

outward, the zones contained an increasing amount of In, combined principally with Ni, with up to 95 wt.% In (balance Fe) in the outermost of the inner re-An intermetallic, Ni 1n7, was one such zone.

The blocky gray 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.

21

The compositions of these various particles, o' specific phases within these particles (denoted by a number), are summarized in Table 2.

Microhardness measurements made on the nozzle body at the 82-mm eleva-tion gave an average hardness of 16114 DPH for four values.

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 surface layer became thicker, the under-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-tion to Fe, Ni, and Cr, in various combinations.

Where Zr and U were found 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 1 10 DPH, essentially the same as it was 13 mm above.

F.

Nozzle E11 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 mm stub of the nozzle remained with the ves-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 upper 145 mm and part of the bottom 38 mm.

The tapered top of the nozzle was wrinkled and =3 mm of the top was missing, but as will be seen, this material melted and ran down into the nozzle.

Figure 60 shows the top and bottom views of the nozzle segment.

The top view indicates that nozzle material had en-tered the annulus between the instrument string and the nozzle ID, and the 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 nozzle.

The cause of the separation was not determined.

The 137Cs activity profile for the segment, Fig. 61, indicates that there was fuel in the top j

=15 mm of the segment and in an area between the 210- and 250-mm elevations.

22

__~ -. - - -

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 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.

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 other nozzles.

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, under the strongly oxidizing environment.

The outer surface apparently was sufficiently hot and plastic to form " micro-folds" that trapped particulate 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.

Examination of the transverse section at the 274-mm elevation showed that the solidified metallic material on the inside surface was contiguous with the nozzle with a composition essentially that of Inconel.

Areas of the surf ace of this material had undergone post-movement reaction with A1.

The ceramic material attached to the inner surface was a loose agglomeration of 23

i i

particulate shards (Fig. 65) that included fuel, fine fuel particles in an Fe-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 i

l cause an indication in the gamma activity profile at this elevation.

1

)

The outer surface at this elevation contained areas of surface scale, about 10-20 thick, and other areas of surface attack.

The outermost part 5

j of the scale contained Ag (11-45 wt.%) and Cd (4-15 wt.%), the balance being j

Al, Fe, Si, Ni, and Cr in descending order of content.

The inner part of the j

scale consisted more of the latter constituents.

A reaction area, shown in Fig. 66, contained Ag, Cd In, and Zr in addition to Fe, Ni, Cr, Al, and Si.

l Silver-cadmium nodules were found up to at least 1 mm into the nozzle.

Hardness measurements taken near the inner and outer surfaces all indi-cated a' hardness in the range of 136-141 DPH (average of 137 i 4 DPH).

This is significantly lower than the hardness closer to the nozzle top only 15 mm above.

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 peak and no metallographic section was made at this location.

it can be as-sumed that the ceramic-appearing mass is similar to the material found at the 274-mm elevation.

The outer surf ace at the =90-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 surf ace be-neath the thick scale was a 10-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-curred. The hardness of the nozzle at this elevation was =190 DPH. about that of unaf fected Inconel 600, indicating that the nozzle did not get exception-ally hot at this elevation.

24

VI. Discussion A.

Defining " Debris" It is appropriate at this point to define " debris" as it will be used in this discussion.

Fuel " debris" is defined here as the material that flowed to 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 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 to be noted, is considered 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.

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.

In addition to " fuel debris," this report will discuss " control rod as-sembly debris " consisting of all the major constituents of a control rod as-sembly:

Ag, In, Cd, Zr, Sn, Fe, Ni, and Cr.

Fuel rod materials would be mi-nor constituents in this debris, and it is difficult to distinguish whether l

their involvement was early in the accident or later af ter the " fuel debris" reached the lower head.

It will be shown later in this discussion that there is substantial evidence to conclude that there was a bed of " control assembly debris" on the lower head before the fuel de.-is arrived.

26 r

B.

Nature of Nozzle Damage The six nozzle segments examined at ANL fall into essentially two cate-gories:

(1) nozzles destructively affected by molten fuel:

H8, HS, and M9:

and (2) nozzles thermally affected by fuel debris but outwardly exhibiting little damage:

L6 and Ell.

Nozzle D10 falls into a middle category that, de-pending upon interpretation, encompasses both categories.

The tops of Nozzles H5 and M9 were destroyed directly by molten fuel.

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-

'4on.

However, with a total remaining height of only 170 mm, it may be as-sumed that the nozzle was melted off in a manner similar to that which oc-curred with Nozzles M9 and H5, and apparently GS.

The finding of what appears 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-zies.

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 mm (D10).

The thick crust patches on one side of 010 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 in source.

What is probably a similar scale near the top of M9 just beneath 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 melted, M9 and HS (and probably H8).

The Fe-based ;cales are barely adherent l

to the nozzles and do not appear to have grown from the base metal.*

Because of its apparently non-nozzle nature, it is believed that the source of the Fe-based exterior scales and the Fe-based matrix in the top of E11 was the fuel l

l l

  • T. F. Kassner. ANL-MCT Corrosion Section, Private Communication.

26

flow that melted its way through stainless steel structure on t' < way to the lower head, regardless of its exact path.

These Fe-based mat-als are gener-ally located in temperature regimes that are between that of molten Inconel and that of the very clean nozzle surfaces at the cooler lower elevations.

It is not obvious why these Fe-based scales contain only adventitious pieces of core debris and not material more akin to the " companion" samples.1 Chromium apparently is not present in these scales because Cr-oxides are very volatile above 1000 C and would have migrated out of the debris during the movement to 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 noted exception of the exceptionally hot H8).

The bubbles formed in the re-mains of Cr-depleted Inconel were likely caused by Cr-oxide vapor, which ap-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-zle.

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 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 surface 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 surface of the necked-down region of H8.

Nozzle D10 was in contact principally with hot fuel j

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 I

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 010.

An es-timate of the minimum depth of the Zr-containing debris on the surface before i

1 27

)

1

the fuel flow re-melted it would be ~120 mm. the height of the bottom portion of the nozzie segment.

A maximum height might be an additional 50 mm, if the I

ablation was truly hour-glass shaped.

C.

Postulated Fuel Fielocation ScenaliQ The di f ferentiation of Fe-matrix debris from Cr-matrix debris makes pos-sible postulation of a fuel movement scenario and estimations of initial

" 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 depths are described below.

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 finding of even thin scales near the bottom of some of the nozzles (not all nozzles were extensively examined for scale formation at every elevation) in-dicates that all the nozzles were likely surrounded by a debris bed that was colder against the vessel and hotter above.

This is consistent with a fuel 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.

This crust apparently cooled suf ficiently f ast to result in no surf ace 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 mixture

(" wet sand") of high-solidus-temperature material (U-Zr oxide phases) and lower melting materials (Al, Fe, Cr oxide eutectics).

Above the " wet 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, 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 j

and the ensuing crust would have been thinner.

At some point in the movement, apparently in the E7-8/F7-8 area, the basal crust could have become suffi-28 l

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 hot fuel to one side of the DIO nozzle to form the thick crust and then en-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 the nozzle would have occurred at this time.

The adjacent and slightly ele-vated Ell nozzle was affected only to the extent of fairly extensive scale formation, surface melting (" pruning") of its tapered top, and melting and collapse of its top 3 mm.

The finding of the Fe-based debris in the top of the nozzle indicates that some of the fuel flow came straight down as it passed over the nozzle, but it was too cold to cause more than superficial surf ace melting of the nozzle tip.

l (It must be pointed out that there is no direct evidence for such a lava-like flow moving in contact with the vessel.

An alternative scenario l

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 l

spot.

The explanation of the elevated melt-off s of Nozzles M9, H5, and H8 would be the same, as would the effects on the other nozzles.)

l l

In the lava-like surf ace movement scenario, a " debris bed depth" can be l

l 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 l

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 600 and its source may not have been the HS nozzle, but rather the moving 29 t

l

debris itself.

Second, the failure of individual nozzles may-have been caused 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.

An alternative fuel-flow direction is appropriate for H5, and perhaps 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 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 by the same liquid level in a stagnant or moving pool.

The same argument can 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-th:ck 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 been melted off by the same height of liquid as HS.)

The. implication here is that H5 and G5 were melted by a downward-moving pool and that they were melted before the pool reached H8.

Both the H5 and G5 guide tubes were melted off significantly above their respective nozzles, indicating that such a moving pool was deep as well as elevated.

Directionally, this flow would not be in-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.

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-gests a deep basal crust and a high liquid level, consistent with a fresh fuel

. flow contacting the vessel, with a direction toward H8 and the eventual hot 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 KS nozzle apparently was not.

The 1

surface debris found on L6 would have been material from the periphery of the 30

i 1

i flow, or simply adherent material when the fuel debris eventually settled to form the " companion material."

The fuel material inside Nozzle L6 is believed to have come straight l

down the guide tube and not from a lava-like fuel flow for the following rea-scos.

First, both the L6 nozzle and its overlapping guide tube were virtually 4

unscathed, and it would have been dif ficult, albeit not impossible, for a rel-atively rigid lateral flow to have made its way up into the guide tube and then dowr into the nozzle.

Second, there was an unreacted fuel pellet segment inside the nozzle.

Such a piece would not have survived in that form in a hot fuel fl ow.

ihird, the L6 nozzle was beneath a control rod, and appreciable numbers of Ag-Cd-bearing particles were found in the annulus.

Fourth, fuel 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-trix binding the particulate was Fe-based, this material would have had a sim-ilar 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 4

material is almost irrelevant.

The significance of its presence is that it 4

apparently generated sufficient interndl heat to anneal the inconel 600,'as evidenced by the relatively low and axially uniform microhardness values for this nozzle.

D.

Etesence of Control Assembly Materials Four of the six nozzle segments examined at ANL were under control rod assemblies:

M9 L6, H5, and H8.

One. D10, was beneath an axial power shaping rod that contained 914 mm of Ag-In-Cd clad in stainless steel.

The last, H5, was beneath a burnable poison rod that contained Al 0 -B4C pellets clad in 23 Zircaloy.

There is pervasive evidence from the ANL examinations that the as-semblies containing Ag-In-Cd failed relatively early during the accident and that the debris from these assemblies deposited in some form, probably as solid particulates, on the lower head before the principal fuel flow occurred i

at 226 minutes.

In this section will be summarized the evidence to support l

i

(

31 l

this conclusion, This material being on the lower hcad 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 evidence, either because the sampling of the "hard pan" was ran-dom and not site-specific, or because the analytical techniques were too gross to identify what would be a small percentage of the fuel debris.

Most, if not all, of such a control rod debris bed would have re-melted when it came in contact with even the basal crust of the fuel flow; possibly it would have been consumed into it.

Therefore, evidence for such a bed would now be, at best, on a microscopic scale and fortuitously derived.

The first evidence that the control mater l tis were on the lower head be-fore the fuel flow arrived was the finding of Ag-Cd nodules and In-Fe-Ni-Zr phases solidified in situ in the vessel cladding cracks in the E6 and G8 boat 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 debris layer present when the fuel flow occurred, there would be no reasonable I

explanation for this finding.

These materials would not have segregated in l

that manner from the partially solidified fuel flow.

The overwhelmingly Zr-rich liquid that contained Ag-Cd masses and ab-lated the H8 nozzle is further evidence for the presence of the control rod debris bed.

The Zr:V 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 Zircaloy shroud tubes.in the control assemblies.

The minimum depth of this Zr-containing debris bed was -120 mm.

The findings of Ag and Ag-Cd inclusions deep beneath the surfaces in most of the nozzles in a form of liquid metal penetration indicates that there 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 penetrated the Inconel nozzles somewhat before nozzle melting occurred is evi-32

l l

I denced by the apparently vapor-pressure-derived bubbles in the Inconel that contained Ag-Cd and other core debris constituents.

Perhaps the most striking evidence for the superposition of Ag-Cd be-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 i

and the inside of the guide tube, debris coming from directly above would be fine particulate.

Indeed, such fine particulate was found on the top of L6, I

as well as at the bottom of Ell. However, whether this material came down di-l 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 masses but only minimally on exterior surfaces and none in the Inconel.)

The material in the cracks in the boat samples and the Zr attack of Nozzle H8 issufficient evidence to conclude that there was a stagnant control material de-bris bed of some, unfortun.ly, undetermined depth and breadth.

E.

Temperature Indicators A principal objective of the nozzle examinations was to provide quanti-tative data on the temperature of the nozzles in proximity to the vessel.

This objective was satisfied 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 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.

33

l i

1.

tiardness Measurements 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 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-tially melted, is inexplicably high and should also be disregarded as not rep-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 the vessel was 133 DPH, a value that Korth's data indicate is achieved in 10 minutes at =1000 C.

Following this line of reasoning, none of the other noz-l zles within 70 mm of.he vessel achieved 1000 C.

It is interesting to note that the Zr surface 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.

2.

Mktastructure 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 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 agree with the hardness correlation.

3.

Penetration by Aa-Cd A Ag-Cd alloy with a nominal composition of 80 wt.% Ag-20 w.t% Cd, typical of the deposits found, melts at ~860 C: Ag melts at 960 C.

Liquid penetration occurred only in the upper elevations of the nozzles where such temperatures would be easily achieved.

Lack of such penetration nearer the vessel suggests that either the nozzles did not achieve that temperature, save 34

l.

i H8, or there was insufficient Ag or Ag-Cd to penetrate, or our analytical techniques simply did not see it.

4.

Miscellans;ous 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 OPH.

That hardness is above Korth's breakpoint at -1000 C, where Inconel apparently anneals rapidly and the hardness falls 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-zles would have been less than 1000 C below the following elevations:

M9 215 mm HS 38 mm D10 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 Al 02 3 and the radial heat transfer path to the nozzle is impossible to calculate.

The observations on p-to-a transformations only establish a minimum threshold of 860 C, which was likely achieved in most noz-zies.

The 1200 C threshold temperature for the Zr/Al 02 3 redox reaction would j

be a good indicatoi except for the heat transfer issue.

It is significant, j

however, that the 158-mm elevation in D10, where this reaction was obvious, is i

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 profiles and the results are summarized 35 1

j

t in Table 1.

It was assumed that the gamma activ'ty was associated with fis-sion products in fuel and, therefore, the results are reported as fuel pene-tration." Metallic debris, essentially molten inconel from the nozzle, were also found in the nozzles, but not tabulated.

Their penetration may be esti-r 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.

L 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, there seemed to be difficulty in retaining it during the subsequent sectioning l

operations to form metallographic mounts.

This would attest to the f riable l

nature of the material.

Fuel material that was retained at the lower elevations in most cases had two features.

First, it appeared to be in the early stages of transforma-tion to U-rich and Zr-rich phases, indicating relatively rapid cooling.

Second, it contained Fe, A1. and Cr in the grain boundaries, indicating likely l

Vluidity significantly below 2000*C.

That would aid the fuel's mobility to the elevation where it finally solidified.5 In Nozzles M9 and H5. which melted off, the penetration was shallow, in-dicating a quick melting and relatively rapid cooling, the phase transforma-tions in the fuel areas notwithstanding.

It is likely that the melting point 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-fled fuel was trapped in the insulating Cr-oxide.

The fuel in the tops of 010 and Ell differed from that in M9 and H5 in that it was trapped in an Fe-rather than a Cr-based matrix.

This reflects two things.

First, 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 surf ace -

scales.

That many of the fuel particles were shards and not solidified in-36

4 l

i i

i situ masses indicates that the fuel flow in this region of the vessel was cooler than the flow that contacted M9, HS, and H8.

This is consistent with a

]

scenario that has the fuel flow coming to the vessel hot spot from the east 3

and southeast and piling up on the far side against D10 and Ell.

(Note that the surface crust and major heating load was only on one side of D10.)

I Vll. Conclusions 1

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 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-

]

clusively, that the liquid was atop a crust of solidified and par-l tially solidified fuel debris that had been cooled below its solidus a

i by contact with the lower head, f

d 2.

Tne fuel flow on the lower head followed multiple paths.

Nozzles M9, H5, and H8 suggest that flows occurred from the east and south-east, but bypassed Nozzle L6.

i 3.

The fuel debris in and on Nozzles D10 and Ell suggest that these nozzles were at the periphery of the fuel flow, likely on the cooler far side.

f 4.

The pattern of nozzle degradation, the assumption of a decreasing-thickness initial debris bed, and the assumed fuel flow directions are consistent with a vessel hot spot at E7-8/F7-8 that was caused by hot liquid fuel atop a progressively thinner crust because of lessening heat transfer to a warming vessel.

j 37

5.

Significant nozzle temperatures ranged from 1400 C (melting) at 140 mm from the vessel at H5, down to -1000*C at 64 mm from the ves-sel at H8.

6.

In addition to melting, nozzle degradation mechanisms were ablation by liquid Zr, intergranular penetration by Zr and Ag-Cd, chemical interaction with A1, Cr-depletion caused by extensive oxidation, and internal pressurization. causing hot-tearing and nozzle ballooning, 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 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 to have been a minimum of 120 mm at the H8 location.

8.

Fuel debris penetration downward into the nozzles was influenced by the temperature of the fuel at the time of entry: its composition, and hence fluidity: the temperature of the nozzle and its ability to solidify the debris; and the degree of interaction between the fuel and the molten nozzle in entrapping the fuel in Cr-oxide.

38

... - ~.

-.. -. -.... -. _,..-- _ - - =

Table 1 - ANL Nozzle Segment lengths, Elevations, and Fuel Penetration Depths Elevation Elevation of Fuel Penetration of Nozzle Segment Stub Missinga Top of Elevation above Base.

Length.

Length.

Top.

Segment.b Nozzle Base,C Nozzle mm mm mm mm mm mm M9 119 254 26d 25 280 241 L6-94 241 64d 0

305 75-H5 107 146 0

159 146 89 max 117 min H8 0

70 51 184 121

<64 010 244 235 57d 13 292 55 max 184 min Ell 221 225 77d 3

302 204 dBased on measurement from either top taper point or midplane bevel, bReferenced to nozzle base.

cBased only on gamma scans.

dColculated as the difference between 305 mm and the sum of the two known values, Measurements of stub lengths for 010 and Ell from photographs were not deemed sufficiently accurate because of angle of photo.

l l

l i

I l

l l

39

l l

l Table 2 - Composition of Debris Areas / Particles Containing U-Zra Composition, wt.gb Nozzle /tocation U

2r fe Ni Cr Ag Cd Al M9/279 nn finside narrle)

Hatrix 29 8

6 5

43 7

Matrix 55 12 5

2 15 9

Particulate 58 19 8

11 3

Fuel mass 88 9

1 1

1 fuel mass 83 15 1

1 Fuel mass 55 12 5

15 2

9-l t6/2R3 mm (inside norrie)-

Shard 100 1

Solidified mass, 1C 83-87 11-13 2

Grain boundary, 1 41 19 17 14 8

Solidified mass, 2 17 54 9

1 14 9

Solidified mass, 2 74 27 H5/140 mm (inside norrle)

Ceramic area, edge 25-30 13-15 1-3 1

51-57 Ceramic area, edge 82 12 1

3 1

Ceramic areas, centerd (35 40) (12-16)

- (40-55)

Ceramic areas, center.

13-30 8-12 7-22 2-10 40-77 Ceramic area, edge 28 15 33 11 13 H8/120 mm (inside norriei Particulate areas 60 30 4.

3 1

l 010/280 mm'(inside narric)

Particulate 1 65 23 4

3 5

Particulate 2 63 12 5

15 6

D10/158 mm (imbedded in norrie)

Particle 1 68 23 4

2-2 Particle 2 77 20 1

1 1

Particle 3 91 8

1 D10/82 mm (outside norrie)

Particle 1 14 62 8

6 2

7 Particle 2 81 16 2

1 Particle 2 75 16 6

2 2

Particle 3 10 77 6

5 1

Particle 4

'22 78 D10/69 mm (outer surface)

Imbedded particle 82 12 1

3 1

I aNormalized-to -1001 metal; oxygen not considered.

bEstimated accuracy is 120%.

Ctike numbers indicate either more than one analysis on a particular structure, or individual areas in a structure, dParentheses identify estimated values for portion of analyzed area.

40

Table 2 (continued)

Composition, wt.%b Nozzle / Location U

Zr Fe Ni Cr Ag Cd Al E11/280 mm finside norrie) targe shard 83 14 1

1 I

Small shard 83 -

14 2

1 Matrix 34 53 8

3 3

Matrix 47 44 6

2 1

Matrix 66 27 4

2 1

i Matrix 87 10 1

1 Surface fold (outside) 74 10 2

6 2

6 E11/274 mm finside narriel Inside nozzle

-9

-85 4

2 1

Inside nozzle 27 71 1

1 Inside, agglomerates (avg) 62 16 19 3

F11/90 mm (nuter surfaggl Outer scale 20 20 57 2

1 I

I l

l t

l i

i l

i I

41 i

Table 3 - Summary of Hardness Determinations Elevation from Nozzle

Vessel, mm DIO Ell-H8 H5 L6 M9 290.

208 29 283 167 i 7 280 140 t 4 274 137 i 4 266 136 1 3 260 124 i Sa 158 12412 130 105 1 2a i

190 1 9 90 82 161 i 4 77 169

  • 13 69 168
  • 10 64 13314 38 202 1 28 25 198 i 8 0

217 1 13b aCr-depleted material, bWeldment.

42

4 A

B C

D E

F G

H K

L M

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P R

NORTH g

/

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N 4

Locations of Boat Samples r

o Nozzle Positions Nozzles Examined at ANL 1

Fig. 1.

Grid map of TMI core showing locations of nozzles examined at ANL.

i 43

[/l' LOWER THREE LCSA PLATES l

' r,

/

E

\\XI VJ VA VJ VJ

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a ELLIPTICAL FLOW DISTRIBUTOR PLATE

/

INCORE INSTRUMENT GUIDE TUBE 87 1/16" SPHERICAL 12"

\\/ SA PLE ELEVATION

'"CO" go ZLE j

f siis"CLAo e 2.s" (MIN)

TO CENTERLINE

~1 0

4 s

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NOZZLE ELEVATION Fig. 2.

Typical incore nozzle with seal and retaining weld.

44

l l

l l

i i

k h incore Nozzle (Materlal inconel 600) g

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Annular Leak Gap of 1.00' O.D. x.612' l.D, about.005* Between inconel 600 incore Pipe and Vessel Fig. 3.

Lower-head area and incore instrument guide tubes.

45 l

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Elevation view of nozzle segment M9 as received. (282582) 46

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Top and bottom views of M9 nozzle segment, as received. (282558)

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Fig. 9.

SEM-BSE image of multiphase fuel in Nozzle M9.

Light i

material is U-rich, medium is Zr-rich, and darkest is l

Cr-rich matrix.

I r,

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pt 4 pt:

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i Fig. 10. As-cut transverse section at 241-mm elevation of M9, showirig metallic and possibly ceramic debris between 5 and 8 o' clock in the annulus.

2X (280685) 51

l l

j l;

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1 Fig. 11.

Elevation view of nozzle segment L6.

(282581) 4.

52 i

4

4 i

I 1

i i

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2 e.

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4 l

ip p i p p p g p p p ip p o g.p p e p i. p g.p p e l

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Bottom Fig. 12.

Top and bottom views of L6 nozzle segment.

(282587) 53

i i

i l

i E

E l

E E

s A

m2 h

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+

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Fig. 14. As-cut transverse section at ?83-mm elevation of L6, showing a porous material in the annulus.

2X (280675) 55

I 1

7 G4' b ',, ',,g /,.. ' '

' ' C, _ -

-..B

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<.A 4*

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e 6

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[ g., -

I Fig. 15. Instrument string and fuel debris at 283-mm elevation of L6.

(Original at 2SX, reduced to 11X. 281570) 56

1 4

5 i

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a os n

S

';i,

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Fig. 16.

Partially transformed fuel mass at 283-mm j

elevation of L6.

3 4

1 i

?y

're 4

.?

l

./

,e p*

y 1

w.

3 Fig. 17.

As-cut transverse section at 77-mm elevation of L6.

2X (280680) 57

5.,

..e, 4

,t.

q F

(

e

_y, s.,

4 e,y 1

2 9

t,

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+

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.=, :,

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.s Fig. 18.

Partially transformed zirconium instrument lead at 77-mm elevation in L6.

250X (281664)

+w.w.

.)

p

..i

+.

j %:.. f,

?

?

1 72 '

3

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c

, 5, s

o Fig. 19.

Etched microstructure of Inconel 600 nozzle at 77-mm elevation in L6.

100X (282531) 58

l 1

1 i

1 1

L,s g, A

..a o

j i

d i

)

b-

,.2 p

g.

pp* R$1% jj a

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3. - x,,

ai 1-m.3. ,s * ,,,,, 3.,,,,,,,,,,,,,,,,,,,,,,,,, ,,,,,,, p,,,,,1 R,. .l 9.. 1 L. 3 6r.,.. 1 7..,... i Fig. 20. Elevation view of nozzle segment HS. (282580) 59

i ~,,meymm, w -. -,.. - h j g s j FL i, 3 .. ~, i '15 l'l8l81' 'I'l'l'j'l'l'l' 818l}l!!'l818l8lI'l'.I'l'l'lil' '18l'l'l'l'l l'l818 'l'l'l8 3 1% 1 7i' '1% 17 i.l.i. i.i l.i.l.i l.i. ii ii.lii.l.i litill.a.le t.l.a.,.s..r.l.4.l.a.i.e.l.t e !,s.l. 1 Top (stereo pair) i 7:n. 7 n pg.y,- .+, y

p.,,, _,.,.

\\ cQ. ? g(g.gl04 ( 4' s,* \\A i: k..'ply';a. y 4 I,. _, ., r [6 , ((#V ? ic Q. j.. g1t31,.,f- - kW O ff't ^ P N.4 5 84li:h* h,,g, h,g,,[,l,l, ' llg;ht, = g, Bottom Fig. 21. Top and bottom views of HS nozzle segment. (282585) 60 a

i i k t i i l l i i l 1 1 i I i I, l x,

  • m: -;;..

Fig. 22. As-polished bottom end of H5 segment, revealing only a solidified metallic mass. 2X (280533) i J 1 1 61

29 2 0 1050 ^ 3 fi Total Cs-137 RetLvLty g73_ vs. PosLtLon (Lnches) ga 900 - mC ls 5. 825 - 0.C Nm 750 - So 22 675 - .8 600 - 4" 5% 525 - -' n 0; 450 - GE f jE 375 - 300 - 83 225 - 2 150 - _e 5 75 - l 5 0 i i i 0 1 2 3 4 5 6 7 8 9 g g= 2 'm4 k = 2 s s 'i U y e Ni ..i a 2 .i . ::n k -+ e E gj ' s:., _ _. _- - - _ y o k h 2 5' .e e e 5 g$ N 5 0 3 b 3 3 o E 3 3 3 E

l t 1 i i i t l, }

  • ) g;.?

a. 1 e-fb. #e;s.;klJM... kfp.' 9 er 4 7 4 7% VV ' 3; g_ .,;- a [ ^ ' V.,, N,,. e l 6f;., i~ n. 1 .~ w' & # > h , 1:g., 4., 4 0$f5 _ I4 av' psf 9 e i r 9% { ~

  • Q pk

? s e Fig. 24. As-cut transverse section through H5 at the 114-mm elevation. l 2X (280530) i k Y j ..y.'. i i i t t' ? 3lJG ~. l l h;*fff t.b - 'y t-o j j j e +* 4 4 L r;;

  • R y.

I i. i Y=%*t j grq' 'o .p. a t 1 : s:. I l Fig. 25. As-cut longitudinal section through top of H5 segment. 2X (280535) i g 63 i ( (

l l i i i vv l$ xi p- ~~ n

  • .r-

~ f 1 i og + u 1 Q l + I n' - f ,. ^ [ 4 t } w n' h:fy,. ? T.? 'g%s &

  • U d

et g P...

  • f#$! ld

%y N ,]9e$ l N SIik%. =[qmy _.h ' g, r Q\\ ,,-r.,/ ~, .,%lQf Q 5 Yi,'l ~ $hf [N8 k:I N[ c.,jp y, 6"th;!';,. M $ r & t! dGA 47 W 97 /5 '~ ?- as.g%i.A,s,.y w,. b; sp h t}.) A*:p'i,p" 't ryirjy,!;4 +,,,, "f*{ %,,.., vg'.g.,, s,h, h, .: + es [' , S M ... way. } - ? '*L i fj .pJ is g 4M-k-)g g '}% A ~ y{h hkS $5?h "JQNll$g(fhh ?,, - J t ( Q r Fig. 26. Metallic and ceramic debris at top of H5. (Original at 25X, reduced to 15X: 280693) l 64

? [?f y . et. -?T w -a ser yyy.y P .y ...;~ go , %e: .py',, ,TL. 4 _ g; f ] s 's ~ gp y y .m%. x x.+ +- x ~ 7 u.e 9.. .Aa, T u .z ;., 3 s.... _.. u.7 f 1* -I g$ nd-.% a- % ~ &l 1 L, ^ S. ..J:.. S sp ; ; A y...;-p,j ~ m., p ;__, f - -, q wig.-L jm fp w - ],m,Q : p,_ m _-,n q. "y,' 41 p.gp .:;- - -[ s - - k

7,

~ = w+w; -&;ay 2 e --,:*^' ~. ~. .,~ ~- >. 'y

.,.. \\l4. +

s. ._ p_; ;, _..,. [@f fp. 4f ~~

y- - 7 yyQy_f'

-r "W 7mgQ2[ *-Ry_p g; ;y;;p _. _.Cq 29 ;, p -- yug ,ygq by n-g4pq ._ a g g; j _I fl-j(7f s . +;0 [I khh I s 't I

" M;W ; W W W;s 8y L4 Y p@xs t mys;ga*Q e ]W ~g e7

- 9 ~ t 341_ '6 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). t

J k i i l l k l l l i i i i s i x (P. F. 4 : 3 w j s._ l-Fig. 29. Instrument string and solidified Inconel mass at the bottom of the H5 segment. (Original at 25X, reduced to 12X, 280635) l l 1 l 66 I

1 i i 1 o 1 i f \\ d J i t. e a j 1 4 i l j i O o /.i / --g I l (a) j .t 3 I g ./* p

- g s'

l

~ 'b. 4%*

f ;* [Q * $ _ s f j! p ?:gg. adi: Ag?qg.;g, Basi,.Q.ggs]yf}; -

- 4;f....,,,

4..m i i (b) f Fig. 30. Shards of Inconel 600 (a) and fuel debris (b) within instrument string at bottom of H5. 250X (280582 and 280584) i ) 67 t at.

hf r=e # 9 g* rY. ..g,y M y'[M' *'sx=,ak.,

j om 4 h%.

T /,0. e n s g;.5 ?~$ n hh, nh[b.W* %/ p. Kt g-5, $/ Ji g L, #g k g Sy;t&)[g,n.n w k.f S S M 4.l,. 4 Yl$wkf%fyM'D, nf Q($'m{<*';,**g. y6% Nw,f m tA u ,a g<f$xh n y,ty*,% ga j:u Wvy$y@'t$.,f^a,;<.;M,!;&s?v n pls ] n f w e,ap. ab {Pw 6 y:f;,.. a Qp;;wO a ~ % f,5,iz$ geb if h ai.,: ?. h.f, nl p kh Apfy%m.qcb&q'3ppu%. fCI, ;e, 'o.A+v.$he %;%vMm. tu;f.Wt c. E %y a v ,* ;< o.;. g;,4 ;. a g n $ f; w, j p ?, f y{ y S Q. 1 yt f p:w. h v as; -Q rmg h o16 y u w y;;;/M.q$.m,% n[;eha. ag % ;&e4 p $ Wp'$ y% y g P q 4,cy y f yQ &(Ph r %-

  1. y ; y,r g

t 2 49 % y;9' t ,4 n% M y p p $ g G e% A;., ;,V' [p W f &y t +:e.Qa #.z'ufu.%eug;%%@wW

,~b WM

%p' l-r; M n y wQ @k;;Q' y u Qq ,y . L 4 cgyb.' N 4 M:w7 My$ ', W,%:n,Y 3q s gri s pf d 4f;g % ".. + i\\ k m 25@V, ey " :!g;g Q m.x <g [J;j. eW }g-K 4 ' _. %y D j n .4 n-r e / s x ,*!Qs:w 3 A li_ 4 Q , 9 pQ ~Qv

  • ~;'.',* ?. %w; g ygA mw+ %.

%a)s mLg r

a 3

, m g +.,.,

'x: ' R A

,Q 9p 2 n @y g ;,%r f ,gg %,y w*%p;; p 3jn;e 7 f L [g. ~f['l i'$y

41

'f} ~ : - 7 -g n3,.%g %sggMp> h s, yn, gs. n l$.d. i<'w's}., R q. h.nw,hy%~p*Y.p y'c'* 3e[(

- [...
  • ,f g:A., y' y 4

Y s .,g .i, %w"$ I fq_ v rl}x0.h:'..p r%c.j* _.. p%ey3 } p, <p g .e._ p, ~ ;y-y.. wh 'w'n, 'x.

  • a

'4.d y g n' ?u ~._ q , f.9)};... ,f].. 6Q*, .a<

c...,

. - y m_ f ' '-f.

h..,

.b !#. p, pfL. , 8* y e,. .,J ,e q\\ 4' 9 - @gt0 #eTb ot o\\ tY \\h no YTe-9% p@

y. % @ E st 9* @~6 N

x 68

1 s

on-J 1 'l .,i' f f Top l'l'l'I' 'I'l!)h 4,117.l, !II'l!II'l'l .15 l a' 1h g Side -e ~. y) 1 cf l St *. ]$,) Fig. 32 O -.. y.- i n , g_ TA ;;; Top, elevation, and 96 .lsplsp slijan splsp splsp splsp ipl spjip bottom views of H8 17 18 19 'gj;;;sP" .-/- 9

s ti Y

.i /L i, ]pg. hk;j 1 Bottom , ggp f-{risl'Itssir ltp i

1 ipjf p rplip iiil>

11 1,1 312J. .1 3 -, 69

) i i j 4 i i i i E e O f -e C I d C i O j '.d 426 CIA 426 ClB g 4 o -n e ,'- f l 4 m o b$N m i FM4< 3 -m o e 1 l 426Cl .e e i s a 1 I. a .N y t I sAmm tf/ l 426C2 j j.ppoippe'in ip'I'l'I'l'I'l'Il o i i i t esaesaseesssae 3 7. j a . 1 c_. 4 i 42G C2.B 426C2C I i Fig. 33. Gamma activity profile and sectioning scheme for Nozzle H8. l Location of longitudinal cut shown only to identi fy specimens, not actual cutting plane. 4 70 l

l( .) I .\\ 1 h h i / J r

I

.D I Fig. 34. As-cut longitudinal section through the top of H8. 2X (280653) k 71

- ?qvNt:. m; L:it-7..E

- e
:w.-ay;s e:':.c n s

.v 3 s ~ pf*6 5h}*[Qe;xf. g ?y j 1 I h.r, i l l ../' Fig. 35. As-cut transverse section at the 64-mm elevation in H8. 2X (280652) 72

- E \\ \\ \\ ~ \\,

Y'~% -

_t, ~ \\c (; 'N

  • y.\\h 1 s

\\ N \\ ../' 3 N. \\ ' :/ - N,' e 4 4 q.. n r r '/' / s 3 N, ) ~ \\ ,{ 7,' _ish \\ .,s)a ~' Fig. 36. Metallographic section of instrument string and metallic debris at the 64-mm elevation of H8. (Original at 35X, reduced to 11X, 280453) 73 l i 4

L i A i 4 \\ 3 I e k ) 4 1 %.. g - V ) a g GP ) s 4.c ss -g; 7 4pphM** ^ k 4 Fig. 37. Eutectic structures, containing Zr, U. In, Ni, Cr, and Fe at the 64-mm elevation in H8. 250X (280462) 74

i s E r 's*"Q-fi. p t .. y, .a - ~. . ns .r __) __.}4 .~ ~- l , 'N - :r- . s m,: m, -~ y, m , [' h~ :m V--,_, ,.e% # s O A h w Fig. 38. Ablated surface of H8 nozzle at the 64-mm elevation. (Original at 150X, reduced to 56X. 280733) m ..y. .,w.w A.c. ] y ss_m

<r.x y ; e s

' 4%gq..W. g' ~.;, *. S '2.,:.KV4f[p w m v<-.& - a;, .,c p .a ~ ~.

  • ,[

v .R iK2G:d[..g g-*. _ y$O,. ~ ^ '^ d ..uf)r % ( 3 q'u:p ; y ;,~ a . ? C.. .e%.-. - - o gR a,:- 4 A ;3.;) s&, ; r&g74: \\ -g ; gy - .~ r ' - -n : y s r.y t M Fig. 39. SEM-BSE image of Ag-Cd particle, "idtA .. )s s ^~ 'M, H.'T[$ghe yyg7$jgj$[.N[s@wd#.m memmb%j and Zr-rich material penetrating f g5 surface of H8 nozzle at 64-mm elevation. ,d w-s, y F ' 'l?b.m'e#di +, *mr- ?44x i . w"' uwn }. Nd. ..+ TV2:@ l "NY'YYYUD.'(#,?k,- ,J ;\\ r 4j .-c ~:&? ~ ' kh $D l s.

t' T

J p

x ko- .~

1 ll
l J

1 w 1 w MkK1%w

3 T1

~ y7

- i

(@g ' j 'M. ): si i l- ? \\ c-S .I a

y lI l' 'l ? l' l ' i t ' l' l'

'l', l'\\'l'I'{'lI.['l?'8.l!{'l?' 1 4 ::"1 F. 1 . " L17 '1 A Fig. 40. Elevation views of D10 nozzle segment. Side view shows crack in nozzle surface. (282578) 76

i t i e i ~pY w <, +s j j .;s s k 1 5( j i.i.,,,i.i.n.i ,i,i..i.i.iq.vl.i.i.i. i.i.i.i.i. 1 8 17 1 8 .i.l.1%it it l.til.17lalili.iiiililiidlefilif els afilslsf airlsleslel#f tfile i a. lisiiliii i Top (stereo pair) l gn@P% i K f ' ~ i hy 6 g g l Y$.i.i.i...i..., i.i.i.i.i..i.i.i.i. 19 6 17 1 8. i 1 i Bottom i e Fig. 41. Top and bottom views of the D10 nozzle segment. (282583) 77

3 3 3 3 3 3 3 3 5 N N b 4_ b = w a O a a a ',m R E E ERj 4 A N ^ A A Al l i 4,_ w l g y A.. 3p y 7,. .r 4, = k$ 01 9 8 7 6 5 4 3 2 1 w O E i i i i i i i i O - 01 Sg l f 5*? g ~0 q

  • Er l

f - 03 $nu \\f eE8 - 04 m I.C SE5 - 05 3?n a aE - 06 S$E g%a - 07 a e - 08 ggg f L

  • C-(

- 09 C g,',: %iM - 001 y .O ( dEg - UlI 12 - 021 SEC m )sehcnL( noLtLsoP.sv ytLvLteR 731 sC latoT _ 031 !52 041 Rgg 2 ? 2 48

e l z z o n 0 1 D e h t f o p o t e h t h guor h t n o i t c es l a n i d u t) i9 g4 n6 o0 l 8 2 e hd tn m f a o0 5 s6 e0 d8 i2 s( o wX T2 3 4 g i F lll 1l l l! l l',il l

.w r,. tty n p,,. r:,@. r o ye P.:, Q i 6 r )0* 7 .J

.,g'ht.p}.;f'['.fvx;vgg3j%'

~ f ' C,h J,$f. 'h;Q, 'j V: I, j,

l. '

^ :Q.g f)) ~,e' Q, 1; , mpqrg.$, goy.... -S a)D lylg.f9% -hR~ . I s. a,, : - -; J [h-6idf N:.,(r' CMAW, IM*f . Jf?$ 9$(S;/.+W if;f b W nJ .N'4 n /$' ,n p y@ - h l 5 e &. 1

s p 4
  • j,y

>s c, ao - 1, c;..

f' f5 Y a > k,

- u. e cw u. k M.y?y,; Gi T j;?% J }s y, p 1:4}} s;q ++c < s. .. c Fig. 44. Typical area of fuel shards found at top of D10 nozzle. r. ma 4 ,}^

,, 3 **

4 4% 7%$7,6 "?ys. ' . 9,. : ? ,,~ Fig. 45. As-cut transverse section through D10 at the 266-mm elevation, showing metallic and ceramic debris inside. 2X (280641) 80 .w

i l I ,;,..s-gag - 4 37. :: a. .e ~ . A s* u-l I dip l i j Fig. 46. Surface deposits at 266 mm on Nozzle D10. l l I r ME %j%iS?;; 1 m.. y + , 2 "

';;.tyr- ;.

~ l. 'r,g @ - .s~*" %? .g. A m i )* 4 w 4 i s { ' jt.. f}fl^ ~- i i s' I. i j Fig. 47. As-cut transverse section through D10 at the i 177-mm elevation. 2X (280644) 81 i ,,,_a,-,-,,en,--<

i i 1 .I \\ j 1 1 i i 4 m,1 ,u n 4 j Y' l l ^ s i

m. ;~

.u goq 7"g 4 n 4.w >.. 4.w,N,, _.f:,. go';:. $ l .\\ ; p,. uj .f u+ ~ 0 4 p, I.f [inx) k;.;' /([dN M 'gch l v. gp),o, ef. +%. ' D hhh S ?.. a 't O t.,o, 2a i.f' w&e::] ~s,h')t L: /::. ,1 Q: p1 r + -. & h Khj)0?bll 4 vn. 4 1y999 i ' &N ,I i l Fig. 48. As-cut transverse section through 010 at the 158-mm elevation. 2X (280646) I j 'I a Y i s ] i 1 i i l i } i ) 82 4 4 A i

=_ ] 1 i 1 I i i; ~ b k l T 9 'h4 - g/ d g C. f 1 i f i '(. \\.' j s [' i '., i(kl A ~ i 1 h l i \\ \\, l [ kh 1 '{ Fig. 49. Area of grain boundary separations in D10 at the 158-mm elevation. j (Original at 2SX, reduced to 12X, 280688) i i i i i 83 4 4

g yy,,- e. - m, 's d i-y

v.,

'l 7 a J} ,g~ 3-5m. c. ,/ 7 . 3.. } 4.- n = ' ( ~ ' c f.d. ,a iii. ,[:/j). ;

  • (

i .3 k ~ 4. .i-3 sl- ' s; a ': g .~+ ) 3W

h0l, i*~.

. i _; l g:,.,. 3 (a) (b) Fig. 50. Examples of Ag-Cd deposits in D10 at the 158-mm elevation, showing Ag-Cd penetration as (a) stringers and (b) discrete particles. I i

W-, s. c5 5 .C m GE

  • f,g.;.% Wjn '

s4 +

  • O Q.

co t m ,.,e h \\. k. g ?' m v*>e # Tw m %,,a. i 5 t { yy TC* y'.

5lm,

+.: e ^ %gu,'$$*ysL- ,,.+ g. s e tv

  • bP g

g /4- /%v.~ y n u s k g .. x o n D (, 4 f Q' g: C ,4 f.V,' m P,.... c.L =/ p ,,e. s ,3j))'N., ..C Ov. sw' ' Na G u a d u \\ ... [ h, E[ I L p e.f. d

%ey s/y; a'

"ob. ,e m $N. i*- 9" e g 'y W (D

e

"g g 5 e 2 u 85

1 4 g %<3: 7 ? .', 3 : 6 [ylf1R;- )[:, ;.(, y 5: W * ?g,1 ', - . g?y=. ? T3 ; .~$ Q v.,._ / U #P: p?. ?$,', f %,+1.,:< 4 y, + :- w a. y h

f. ;

I;'N I hh '.,b[d "d ., f:, : \\

  • Q ' ;~ y.

fi ~. y,. 3, y, R.g+3 ; wt 1 .j; n, 2JQ... /. t'= 4%., (J:A 4.l -3.. '.. %.. 1* f'p- ), .i (e., 's,L s. e .c. i wms,,. a - Fig. 52. Area of grain boundary separations in D10 at the 158-mm elevation, etched to show possible second phase and internal grain structure. 9X (282558) 1 86

- // v,&l 7 S[i ^.,'"S ,q i;U tu%.

  • a liO

( $;cl0f:% 0 jM "y l , g t. }' ) 1 '\\1 ; e ', -'g s.,- il >

, "i.

n . i' y . y w ;+ t. - y-S W. 's'. 5? s. 3 i Fig. 53. Portion of thick exterior deposit on 010 at the 158-mm elevation. A fuel-containing area is on the left (arrow). (Original at 25X. reduced to 16X, 280694) 87

. U,- ~ ~ ~ }. .t ,. ' x',p.. .Jg 3 Y \\ t-ls. w m r. 4 %[ s, \\ p. ,,, y; ).;--- Fig. 54. Examples of Ag-Cd in Inconel at 158 mm in Nozzle D10.

4 i .i e 1 1 1 1 4 i e:.y.yg.rg.,4y73; ? S i l yY@}~;'it' /,t[' u; n

  • j

$j g\\' 4j.,,k: {.,,, 1,{,s 'Y ' 91. y, %.; n ,;b ~ l'- 1N. 9 l lA s4g)t 3 +lx' k'{ ?. ; q 3.'q bflj'p,j,ld{hVI?f?.N){s if f Fig. 55. Segregated U-rich (light) and Zr-rich (dark) phases in fuel particle in a deposit at 158 mm on 010. 89

>g e. s 9 n,. e Q, 5 } t -) O .3 ' '.0 . l, l h I i,,/ ,, ?

f.

' J' Si: ~ %g f Fig. 56. Instrument string at 158 mm in D10. (Original at 25X, reduced to 15X (280673) i 90

I ( i 1 4 1 -.,ls,. h l e n. l j'.t .s l

  1. y'WQ

~

h. o?,.

i I., .[g' A a

r.'

j l a f J .q t"fs' e i 6 ) l a Fig. 57. Melted Zr lead wire at 158 mm in D10. Phases include j Ni, Fe, and Cr back diffused from the locally melted j inconel sheath. 250X (280669) i 91

c en

c..

r -S

).,

.? k. 4 ..y _, .s %t 4 r q' aq. p. .g y \\p,,, bi .a %Q' Q ,;, j,g ; -s Fig. 58. Layer of debris on outer surface of DIO at the 82-mm elevation. 250X (281852) l 92

1 i 3 . S *, i 4;;i S$$ l+(w,!b h.t ' y.. .ft! p> I_ [Mg.: "A .y di?j. p.+A '/ ;'dd 3'9 f +)1,dwy?L4$. i c % T,4 J +: 1 l 4 {

n 4..

l s. I i 4 l i 3; j a3 .l 4 j k i [ 's l i l h.k

T t i

l , fp5, p h' R 'r i y-h ~ .f ~; s .c i /* 1 1

r?

s f. .( x2 ~. -.. 1 3 4 4 g gy 1-- . h $) l g (,s:. :... - M M ~. 2 j...t........Ll...l. Fig. 59. Elevation view of nozzle segment Ell. (282579) 4 93 1

m j ~ a y \\ 't. k!' l ,s. PK., $MAEM {#!:'ag yh! A, 4.... i,ii.i.i.,i,i,i,;,ivi,,,,i..;.i.i.i.,.ni.,,ii.i.i,,,,ii.,i,ii.i.i.i.i., . l. i........ l... i.1. 1 ..... l....1< ...... l... i.1

7. i... l. i 1<

1 I.i.,. Top (stereo pair) S he ~~ 6, j i / r .t / ,. J esup - m w &.l3l'Ijl',3', c' 8.i,.i.,',"DJ,":;JuaL iggf - i y 'l3l!. Bottom Fig. 60. Top and bottom views of nc zle segment Ell. (282584) 94

P S6 i i 140-(Lncheg) Total Cs-137 RotLvLty vs. PosLtLon 130 _ 120-110 - i I n 100 - t ..c f 90 - i m i 80 - f ? I t 70 - = 60 - C 5. 50 - C 40 - y 1 + O 2 30 - J ? o" l 20 - E { ' ~ l J l f n i i i i i i i i g 0 o 0 1 2 3 4 5 6 7 8 9 i =. 1 a i O n m i - r.J ~;,3,z. $f, n -w s+, c e 'M ~ ' ' ' ' g , as 4-2 g,._ ~ x x x r A N. 2 A A g B N P O M h M o ,4 6 P m m L C - -? m m u g N m_ b b w i ~ tIf 3 3 3 3 3 t t h I i i t

i 4 e 4' l f .? \\ /1 - fti 4 n 1 I r

l i

.49 l 4 i v, Fig. 62. As-cut transverse section at 274 mm and longitudinal section through top of Nozzle Ell. 2X (280522 and 280528) 96

t. d[ . t.f ,e 'g' ' '?' . $j ? ' *}:.,,, N._. . ~ 4 t- - W, s.-.. j -

  • q.;,. *.. f ;,,f,

.d* g, -n- . _7 -....: j:N

  • jj. : s. -. I '

's N'. 4 n y: >%f I, ,~ .in- 'a a5;g:.,:h.. ~e y .n ..s'7." ' 'r . 4,. ,, *) ?;.

    • t

, h, e ( f(? g. ' '* 'f T ' O, - p Fig. 63. fuel debris in the top of Nozzle Ell. (Original at 25X, reduced to 9X 280636) 97

J*! $(F *J')p g' ~.% .g RT, 4 p..;ga4 2j s. 1 q ;. J9, yf ' -.g.l yy:;}

A at.

y;f:'?- L'y %c W]: p:gg $h >;:gy J 2 3 >h,!gh;up y,c ,O K, QMMJ4M4 l} V', u yh.$K;; Qi' 7 . $rfy: g;;<~g:tsj%2kl yh;L, sy;.yy,.t* if 3p : g '.: 9;1 + k r- .. %? c }j.ll$. lf 2IQl~>QQ ', ?:

!: I. { c.[p[ J,

l , t. e,^ R, y r rg; > Fig. 64. " Micro-folds" with trapped fuel debris in the outer surface at the top of Nozzle Ell. .f.~' ' 'fs g f f nJ.; 1 e, ' q y, i. - ljg, i - ~- I b. A 'A?n..&k l Fig. 65. SEM image of fuel debris attached to the inner surface of Ell at the 274-mm elevation. 98

i l l 5 1 l i l ~Sk'l$ i? $f5W V

<-c; 's)a,p p/.4 s &,

'-w o? . ;' - t s;g 3 [ 'I_* ,,, V.f'. @ 4 ',{ gj ' ' %Qg.(

y y w,.

x; .o -98 . ks ~ 4 ,. a e-1 1 } I a w _p-i a, Fig. 66. SEM image of surface reaction at 274 mm on Ell. Ag-Cd nodules are evident within the nozzle material. Il F I t Y tN ? f. Fig. 67. As-cut transverse section through E11 at 220 mm. Small gray mass at 3 o' clock may contain fuel. 2X (280525) 99

i l l i T b h b'

1..... J '.-S
,;sT i

l l l. i Fig. 68. Flaking surface debris-bearing scale and surface-adherent scale beneath it at 90-mm elevation on Nozzle Ell. 150X (281913) "y ~ *^ s y_ .( Q~ .( Fig. 69. SEM-BSE image of scales shown in Fig. 68. White dots along 10-inner scale are Ag-Cd particles. 100 c

Vill. References 1. D. Akers, S. M. Jensen, and B. K. Schuetz, EGG-0 ECD-9810, Companion Sample Examinations April 1992. 2. Phase 4 Status Report, " Removal of Test Specimens from the TMI-2 Reactor l Vessel Bottom Head," Project Summary, MPR-1195, MPR Associates, Inc., October 1, 1990. 3. G. Korth, Presentation to the Project Review Group Idaho Falls,10. May 12-13, 1992 TMIV(92)EG03. 4. Phase 3 Status Report, " Removal of Test Specimens from the TMI-2 Reactor l Vessel Bottom Head," MPR Associates, Inc., April 1,1990. 5. R. V. Strain, L. A. Neimark, an J. E. Sanecki, " Fuel Relocation Mechanisms Based on Microstructures of Debris," Nucl. Technol. HZ, No. 1 (187-190), August 1989. 6. " Video Inspections of.Incore Instrument Guide Tubes", TMI-2 Technical i Bulletin, TB-89-07, Rev. O. Hay 23, 1989. ? l l l l i 101 t

IX. Appendix This section includes the descriptive data sheet for each specimen examined by metallography, SEM-EDX, or hardness measurements. A-1

Date of Sheet Preparation: //[92 OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: gfg/g/ Sample Source (check one): Vessel steel f Nozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core Grl Lo ation: Sample Location Description (attach diagram if necessary): Se le is from /he kvefed & & lAe do2 /e a f -fhe. .zes m m e/evaRost. Say/e comes o.D and.z"D surfaces in. a fransvesse Vieu). Examination / Test

Purpose:

/, yeferr>,,;,pe n afure oA eny sueface A'wds sn oz> aas xx .s urfkees/

2. khurmine ce atfrb ~ o/ noz xle rna /cria l deae' Surfac e.

Examinationfrest Technique and Formatting: ple/=# and SEM-Epx. WI'*/phyf okyyAs, SEM im9es, and Y-ray sph. A Examination / Test Observation or Results: // arc / ness */3 /67.f 7 M. QD Botd ED 0.6 ~/.cp ff shd' /Byek cA, in feracw wt A base m e taf. sur+' ace s, //o coeyst lv'ex!c/es so.n e nort -uniform in, l Byers are and Al [oa/asas ar/w u-2c puat s4acds. n.f S-A~/ /.parfwp u is z . seo. /ocaAons Fe - etcL WUh cd a d ofAer.s ric4. tu. A 1. *r Other Parent Breakoffs Sampi Log Nos.) and Purpose):26ASA CSEaf, M A M $""b " 42442A/ bf 426A Comments: Add additional sheets if necessary A-2 j

et sheetPrusm_, oste ation Project mary Sheet TMI 2 ess lInvestig e Sum V / Test Sample Examin tion Other (specify) OECD a / g g6,42A/ VNozzle ion _ Vessel steel ,_,Compan Sample Core / l / Sample Log No.: k one): _ Guide tubePrincipalinvestigator: O Sample Source (chec W hA77 /,8 A Dl lAe ion: PerformingOrganizatWGffM diagramif necessary :l' 00%2le s/n g [ ) u yQy1/ -/ cription(attachaen & Ars4mm,r / 0 e / SampleLocation Des from / ants vak. Gri is Sg,,,p/e ele s m sse. 283 m and' fu / me

clebris, e

fue./ and Comf s/Non-o$ aQ e k gy,,gned fairiesf. / e: of insfr maleMa & amination /TestPurpos um Compi/sk insu/nfo r of c 8EAl~SX* et-am te and Formatting:and A hamination/restTechn //grerff ique 2:-s/ ryte/s or Results: bexb, f. / C ation hamination/ Test Observ ki r'ef Sere. A/S/ (SE/r/ }a dness /24 A58 (? tat ) and Pu 'teGSh426 ose: N2 ffs(Sample (LogNos. d / SEnf k 5,4 Other Paren Breako t6 JEM hardn r e-4nAs nal sheetsif nec ments: Add additio Com g-3

OECD TMI-2 VesselInv Sa Date f Sheet Prep Sample Log No :mple Examination / Test Sestigation Proje o aration: Sample Source (chAg um ggj mary Sheet eck one): Performing Organi _Vesselsteel zation: Guide tube Ane acr/r#5 _/ozzle N Co mple Locatio Descripti Principalinvestigat mpanion Sa _Other(specify) mple is fron (attach diagramif nA.4. /Ve, Ma n or: Sa Sa ")"mple Core af Me e der ecessary): [* om 77m e e le v n sarfa m e u ce of noz2le ExaminatiorVTest Pu A/022 rpose: dep/et/s,ic/ cts /fuC/ure m estd hardness. A 9 N'~' y Examination / Test Tech g MeAr# nique pkc Paphand Formatting: s O i$n / A v dp4kpS e E g, a ts, SEM-EDX, a d W stess p Examination / Test Ob me n ur& e.V.N images as for' ntkMSfitteM n or Re x spec 6 5, ud a n servatio W9& es'5" sults: , Se 3 A.S*B. /@ t lexf )0</A. e 42 6 Is i //o discent6/ /5 NN, Are/u f o n d' a no e fu l radu fsuedr et% mea n s Other Parent greakofff?agule,SgX/f e ee /s sure e raa .s yee me.fa e p. $3 A**G ju, w a da&' G'. Ao ,a o n yWASk2As (Sample Log Nos) an 5 v.s j in [s [r$y_.g,., '"" e' ekaG(ed a Com ments: / W ),. d

Purpose:

j it/ -/24

  1. .26A/

u..fa. ASB(4*d're'8'(SEN c4, / sh 4.26 #ad A5d6 Addaddition lsheet A-4 a s if necessary

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g 46,42A/ Vessel steel t/ Nozzle Other (specity) Sample Source (check one): _ Companion Guide tube Sample Core Principal Investigator: Gr ation: Performing Organization: Samole Location Description (attach diagram if necessary): sai,,p/e is frem. cen/er of nox.2/e af /Ae ,285 mm. elevaL, Gr'ai:.1s ins /rumen / s/nug and' fuel messes. Examination / Test

Purpose:

h/ge,,gg e ap/gge o[ [ue/ c/ehris, i N'o r insu/nkr /7?BWi&Y gnd Cemfa of ins /rumen4 tJIt'eS Coor7pfhk oG c ereas t*c Examination / Test Technique and Formatting: bad SENSX A ,;:g/ 77pe/w//graf f Examination / Test Observation or Results: See. re g t fed p./o

  1. 24A/S/ (SEN aiwi and Pu ose:

Other Paren Breakoffs (Sample Log Nos.) d Et 1.2f> AS8 (? gat d'rsesaf f MeGS ll'a dnes f,Zf:,4 5,4 (sf~/t/ du 4nAsc65EM) Comments: Add additional sheets if necessary A-3

l Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: gggg Sample Source (check one): Vessel steel Vhozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: ' Sample Core ,4,w-acr/rics z.4.Me, wark "*ff"; Sample Location Description (attach diagram if necessary): Sample is fre,,<. eu/er. surface o f itezzle af Me 7 7 m.n elevay%. Examination / Test

Purpose:

Abz2/e miems/rachte, na hre

  1. '"d""

depsi/-s, ar,d /2ardnesc, Examination / Test Technique and Formatting: Me/a# t aphy,, spief-EDX, ancf W-Op/?ca pb/cgrap4s, sEM images and EDX )Geef3 b d Lv dness messurn e. fs,. Examination / Test Observation or Results: };pf ntk::/oSl/ttclcere, See l'kb f'lA* flatt/ ness is /@.t/ 5 NN, Asch 4% rn e a $ " '1*

  • d " 0 't 4.2 6 A C B Afo clkemvYe SitWMC lGyer*.> +/o a
  • p2~/n u//q Zncon/

i exidafier proefucAs pies.: rom e fue / pa Ha v /c,, s.6 x /40,u, wv. scc /(~,W, 4ss fe ' t.J-Zr hebeaWe d in s nele c4, Other Parent reakoffs (Sample Log Nos.) and

Purpose:

fE6A/8 La"*'"ess,426A24/ (12!=N.), f26ASBGia'dtress)(SE# 3ao'f.26ASC(%4) Comments: Add additional sheets if necessary A-4

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g ./J Q g Sample Source (check one): Vessel steel VNozzle __Other (specify) Guide tube Companion Performing Organization: Pdncipalinvestigator: Sample Core

4. A. Aeanark

fy "*" / Am.-ac7y.r' ps Sample Location Description (attach diagram if necessary): e. Is fraort inner SCU~fBC2 "S *

  • 2 lC e/eVa'b'on.

Bb lbe ~/ 7 m m. Examination / Test

Purpose:

YBPdness Examinationfrest Technique and Formatting: DPH Examination / Test Observation or Results: /69 2/5 W//, br/ud eneasuNmeh //& ness taas a 426ASA, Qthgr are Breakoffs (Sample Log Qos.) and

Purpose:

-(J4A/8/[SEN ""d 426 A5e(SGM )($6M), 42MS4 (%e rj SEN, Adness} e >426A1A/ h3 Comments: Add additional sheets if necessary A-5

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examinationfrest Summary Sheet Sample Log NO.: &ffg)f0 Sample Source (check one): Vessel steel V ozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core kAll.~/WC f E M /,4. //GAn a/~$ Y Sample Location Description (attach diagram if necessary): is from cen/er of no2z/e a/ /Ae Say/e 77 mm elevabin, Eire /ades 4ozzle _TD avd ittSham en -f S/P/T' j Examination / Test

Purpose:

I k fnvmine rya /um 3 f m e/irl/l*c 09 mest/ InG"""lj degYead',u> ires.a.,d me4 fury'caf <tafun a f zD surfac e ast/s cede & af infrumed Examination / Test Technique and Formatting: M e fe /4 e 4 as d qphe,?p$/Yyag, sad-6:DX.sen i:nyes, aad Gbx sfed Examination / Test Observation or Results: f8 Xl, f /. GCe-l Nos. and

Purpose:

/164/8/ @/// 3ac/ Other arent reakoffs (Sa le L 4(heraness 42M.5A'il (mef Sfff, dadess), har es 26h2 / 4.2M5 comments: Add additional sheets if necessary l A-6

l i l Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: A ggf8/g/A i Sample Source (check one): Vessel steel / Nozzle Other (specify) Guide tube Companion 1 Performing Organization: Principal Investigator: Sample Core i l ANL.-Acr/zps L,4. /VeAnarK

  • h*f*";

Sample Location Description (attach diagram if necessary): Sam is a franswese see.fibn. af /Ae 24/m~ p/ee/eva.fru a/ /Ae oufer sue See of /de @22le. Samy e cap /ures moHen. stosx le mnkrie/ l an af &=fy .surfaca alebrin, I l Examinationfrest

Purpose:

sad ce m it k D e fueh n kse n afuew e f ene /s/l4'c ,$ frug.7 cre, //,pec/ngas k in f)e f BSes i Examination / Test Technique and Formatting: SEM ~ ED)<, ns e loWy ra,o A. f y*c.s/pAoloyyAs, sest images, EDX sfe=fra. Examinationfrest Observation or Results: Aff/,/ sse cag/af,, ere< mere er.s i s C,- /e/eal Zmo,eef(93M-4 sre-yaye,/ bu44/esfhsee Vafr-eleycui/e/.s'/ruefares du/ 0.2 de,), Abble.s con fai t

Sunel, Cen 1'sth Ag, Caf,frr & A/ padSc*j Ca aad 77 oIso "A/n= lee, o e ma fr/x
  • f C ~~ '~ L Cerannte 4

is a ? pare 1.slaa d's a# ll-2e s.y ci. _gtpe -yA/d Ma f code /*S f as e (Agd-[tt,g}ues

  • 0. //pr/nm of n/ZW /eo h

f 4jg Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

426 3/424 (SEMh 426.323/ (SERF <wd dardnes.sb Comments: Add additional sheets if necessary A-7

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examinationfrest Summary Sheet Sample Log No f3/AM Sample Source (check one): Vessel steel ( A fozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Cora Grid Location *- ANL-Mer/IPS Lai4. A/e/ mark 49 Sample Location Description (attach diagram if necessary): Sem is, a /oiig/A<dinsf se=&n Mroag de & p/e o A stozzie aS Oe mIQlane. Sample Caphtrrus nozzle and core Sur face $'oe one .Z~.D clebe>*s is. cenAer, and fce-of n/Sr'ruon ed Eex& /ead. (See Fiy. 8 / n. Examination / Test

Purpose:

Dekemine spa hre o f rne lad $c and cerax/c. A J ases. Examination / Test Technique and Formatting: N8la$ /'B 9"d SEN~EDX, f A p e/o and SEM / mages and EDX.sp, 25x o i Examination / Test Observation or Results: See /exf, p.g. Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

ness?.444 (5"EMD,rd hard'nessh -424 B2B/(SEMaddevd-426E4 comments: Add additional sheets if necessary A-8

4 Date of Sheet Preparation: I OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No Nf[28/ Sample Source (check one): Vessel steel Vffozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core ,4,yz.-yag,z/ ;ss z.,4. Ne' rart

  • '%c)"";

c Sample Location Description (attach diagram if necessary): Wansverse mv6br a/ ouv4er-sueface af /Ae 38mm eleva-hk. Examinationffest

Purpose:

kNtm/se // a/ut-e of Da} St.tt-fate WyIh Bnd slo 2z/e

jgedness, Examination / Test Technique and Formatting:

SEM-EDX an d' DfW b"N5s, Examination / Test Observation or Results: //ardsss /s to2.f 28.2>PN / eyer,; e.s-xopjric4 m Cr p*mobEf " f r/ tit surArca i sxide. Occastenaf de ss/s of 4/ Q/,0,;>) k /uyer: raorH4 6 / ao/gboundya .%ne enk/ iva' ma ero/.s in foye r, Base ma/w/ is Inc. Seo. Occastoo<a f grain f M e <*mf'r4'o n &.Z~stcone/., 6 / bav/ base ne/,/3 yrehab/y% **/ $2ses

corkVes, as/rsdo.s se s f /4
  • Other Parent Breakoffs (Sampie Log Nos.) and

Purpose:

426f/4/A &EM aod bat l ness), 4 2d> SAIA (SEM) f Comments: Add additional sheets rf necessary A-9

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No. ffC/A/ Sample Source (check one): Vessel steel Vfiozzle Other (specif ) f Guide tube Companion Performing Organization: Principal Investigator: Sample Core 4y. gy/rp5 4,4. Ne/ mark. )Ej" "; , Cample Location Description (attach diagram if necessary): on., z%. #1elYa,,d vy *suefaas. /brott L ihdha {.Secbbot. l 0 n te. cap uus s Examination / Test Purpose

  • bI*

Dederinine /? B lar-e 0l f5

  1. 't-s/ /Ae ba'e surfaces an d

/Ae es,iryiasidam /ffelal-Examination / Test Technique and Formatting: SEM -fDX. SEM. images and E.Dx pc.fra,.DPH nicasu r-em e s /-s, Examination / Test Observation or Results: .See text, p. /s. hase mehl was mma / "DPH was Mas 73 .Znc. foCO.

  1. 14 C/42 (m eldj Other Parent Breakoffs ( ample Log Nos.) and Pu se:

f2G C/A.nAC(met 424c/A38Gne 424 C2A Css ess ), 4.2 6 C2.D m e t. and SEN_. -42bc2C / bar Comments: Add additional sheets if necessary A-10

l l ) Date of Sheet Preparation: l OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet t Sample Log No Uf,d/M Sample Source (check one): Vessel steel tAfozzle Other (specify) l Caide tube Companion Performing Organization: Principal Investigator: Sample Core A NL.-Mar /76 4 v4 We/ mark Sample Location Description (attach diagram if necessary): Fheu.da transvers:e seckoit. oS insfrum*d s/rian

+

C2A6fM) Aara'n ess 426 et C2z> (me f. sa/MM) 426 C2c Giars' ness, -/.z Comments: l l Add additional sheets if necessary l l A-11 l l \\ l .1 Oate of Sheet Preparation: OECD TMI-2 VesselInvestigatio. Project Sample Examination / Test Summary Sheet Sample Log No.:,4 ,fg g/g g Sample Source (check one): Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core Gr tion: g, g g g g g,gg Sample Location Description (attach diagram if necessary): Lcirp;A&>,af seeAu o# ces fra/ Adeumed sfrig ZD suefice a f M e. ~ 90 m n > eleva-koa. Cap /uces.:ro//dsi4 ed debris (%a'" .S/ rih stefah/tc) rda, flHer side of e-on du //. X"%*d co-aird ort e i4 $2e ancf cese fathed sVts/rumen{ /eads ll~/l 0"l *b cardat/ duriq yeparafion. Examination / Test

Purpose:

Eerantfc /773l era 2l lA $ryj,y y// h /desy}// ad /tt.S/rumen /.Slr/stg, @ntru./u $ futeen rio 21 k .freparen Ab*t cod nol Caf rt V e t', Sant Examinationfrest Technique and Formatting: Me/a dy' cuphy, L /o 2So~ X-Op//ca/' p2daX, grey c Examinationfrest Observation or Results: bl f25 04/' *bI~ .6*/fRc /u t-es th>tyfa/st ff/Mh y Ae/ds, o.sd areas e/' exidizeef n7ekl o f.sfraefuees /o r%se of f2fo C2A Am;/ set Gcos.:nbesf.s .sg es L are .s> // d % ' 1 %. t o o e o i da s.1 - /N U,Erj attd its/anals o/ & - 4*e/, ifQe,,Cg,37.) i arent Breakoffs [ Sample Lo Nos.) and

Purpose:

/24 C/4/(SEN MM3rd-Other 42f,CtA2(dne)s,S 2g c74 3 3 gngg),,.,(,g c g g p g g f nre,c tress 2C/ (%ar . f26 C2 D rme A and SEM 1 - 426 Comments: Add additional sheets if necessary A-12 \\

l Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project i Sample Examination / Test Summary Sheet Sample Log No.: & g] f [fgfg g Sample Source (check one): Vessel steel VNozzie Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core >4NL-Mer/ZAS

1. 4 A/eirr> ark
  • 'yy*" "

Sample Location Description (attach diagram if necessary): Traxsvere.see /p>z fem FAe caen lev ~ o A M*2 E le 9h hke

  1. 1. 64 mm Glev3Ne** C burec/ /2o2zle E/7ner-Ster-face. Lt)/lb Jo/t'ab'k' tryefaf age /M$f l

c?MW nVit ces.be& f eCA *b kke Con WwY, i ExaminationfTest

Purpose:

MBSeM*l IA. C BMC / spa // k exams'ne $rr}/u.s itozz/e a*t d As s/tv< men l.5/rNy be/Weexmaa herd fraxsweseY su,/ / 9xnu l lowever'/in a/h,te. som /ong//ue Examinai[on/ Test Technique and Formatting: k k 2 SOX, lb rany s 3 i Examination / Test Observation or Results: SAcacfu a s ide' x,4 caf 6 A4ne ir du cz4; fossi.bly ina&9 sue /kces. Miceos/ rue /ures i BlSo .s/rrsi/ae 6 Hwse-tr 4M C/A3A. Other Parent Breakoffs ((SampiqLo Nos.) and Purpfo-e:.g ,426C./ 2 mef &C./A34 mei 424 C2A MCS6)1 ) 426 C2C / Cfrardnes)s,, 4.24 CRP (me t and SEM l l Comments: Add additional sheets if necessary I A-13 i

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: A fff UA Sample Source (check one): Vessel steel dortle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core ANL-AEr/res L,,4. A/e/mard' '"jj "* Sample Location Description (attach diagram if necessary): 7 rasswer,e se::.% fro,,,,iAe een kr o / nozz le heAn's barfiaIMiAed') had af /Ae 64 mnt eleva f*on. C insfrumen +.s/r/ anh nozz.h //scknee surface, Gee-me in annulas, le Fig. as ir wi.) Examination / Test

Purpose:

.1k/erari:,1e nahre s/' me h/h delvts in. H e ;r,,natus. ExaminationfrestTechn ue and Formatting: ) Mefafs' ey an d SEM-Eb:<. Aca/y 6,9rayLs 6 25ac.; 3EM Mages; 0,c: EDx spec.Na Examination / Test Observation or Results: See le-x/, y /S-4, 6C/4/dEM hd M*M-Log Nos.) and Pube: 4M.C/AaBcmed Other arent Breakoffs Samp AW'S > 4.26C/A2 me 426 c/43,4 e 4.24 C2C/(&a e , 424,C2D Gne and SEM) Comments: l Add additional sheets if necessary A-14

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g gff Cg / Sample Source (check one): Vessel steel dozzle Other (spech Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core Gr ation: g j gg,, g Sample Location Description (attach diagram if necessary): fr~Brrsyter:S:e 3ct:f k of ou fer-riozz/t 5ur-Sce Bl /ke 6>4 mm e /evafh, Say e cap /ures l ios S " /2 mm o f Jue face sa c( ex,teau ds m j o m ot

42tle, Examination / Test

Purpose:

Nar-dness ef /70ZZl6. I l Examinationfrest Technique and Formatting: pN "f. Df9V M7*?asuremen /S j 6'. 6 X y Examination / rest Observation or Results: r4ver%e of (o me neurem en f S LJBs l53$ $ 426 C/4.54[~reOfose: #24df4/N#M48'/"*h Other Parent Breakoffs (Sample Log Nos.) and Pu (Inebk 42.6 C$) D Go,e / an d.1iC4' )426 C2A (/d:nd, 42 s CM38, 426 C/A3 6.,ee' Comments: Add additional sheets if necessary .A-15

l l l l l f Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g//g g2' f C2,D Sample Source (check one): Vessel steel vbozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core ANL -brr/zPS L. >4. A/khmerK

  • y " ":

l Sample Location Description (attach diagram if necessary): W3"VeMC See/rbn. e f.:sey enf s/ ou fer-noazle CurfKe I a/ He 64 mm efeva kon, su eface. erea is one of Severe abla// cot. b eherm/ ore ita/ure of /skTleri.nl *^ 'f aZzle SurfoMe Examinationfrest

Purpose:

BMd h> elucidirAe m e c 4 a n t's m. o/ Scirface a Hect, Examination / Test Technique and Formatting: Ale /al/cgrafy y SE4f-Ez)X analys/*,- to swx, sEM images, and qatcayfoyyts avx -yesca. (See g A6 of /esd.) Examination / Test Observation or Pesults: ,,e ne. 4oo. u%sa meh/ 4as irom.,,, / co Y sifie. o/ surface by er Mal 2e.ned AC fewiys/ ceas/;/ueafsMtchosc fe, ce sad tJ freserri smnifer-am fs, Ze cad;e f 4 6mp in varios from to o in byer 4 in soy <: A*ca.F/y W* hk b 2r J.Zir /* N r u a fa rba / R// wil4 s-por ear-w/iner=kJCd, y:Cag n 24 .u, s/,, (~f12 -2a,,4 2,, in 2e - N'i surface aHe y', o k-cat Gnet,), 424 C/43Afwaf ), 426 C44(Sf/fMe d Other Pare $t Breakoffs (Sample Log Nos.) and

Purpose:

fa6Cfd2(~ eO,,426 m .pzs cz ci (har dness Comments: Add additional sheets if necessary A-16

1 Date of sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: A g,2f,f)/E/ Sample Source (check one): Vessel steel Mozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core Gr lon: g 4 g, g,g g g Sample Location Description (attach diagram if necessary): l.ong//ual/nal Sec//m llW*"8 d fxianafe mihh*

  • elevaho., he/ow & suefwe. 3*ymm+

khe ~/as mm Is 0xrm

  • t s'g k.+ " S i el e o.[ nozz.fe - a,s & inc /u des &

oufer-surfeeg., 6ee of Arse-gec:,araes across 0 trozzle, Examination / Test

Purpose:

befer,,,74, ny w of mela/'&c mad ce m ppa arses. i Examinationfrest Technique and Formatting: lLs N 2W* M / 2.Sx an M BDX y, Examination / Test Observation or Results: [See dec/,,g. /J.) /s essm/re/l Cc-led zo,. too. Hammas M e /* /PEc ( A a c e%Lhles' m.s/cucfuee, Mee/k-//ke ofe' /es ) sfrue. Aces t assectafe/ ynarwHy wiM bu bWes,.>r.e & ~t tc.L 6 xile ?), 3a66/es w fes,, vpe-Aa./'.Wru c M., a=~e * / w Lav 4. . c,, e ~ e - a..,s cc-a - w a,asew*Med.n ~ a.d 2r.-r,a/a. chases F*ae/' pMones s*4 U tva e T Jn.s u..

  1. 26 b/82 6.,e d Other Parent Breakoffs Sample Log Nos.) and

Purpose:

426.Df B3 Cm ef., 416 pl B4 Cm e / a-d h ardness). Al/ W SEM ex am in a ton. Comments: Add additional sheets if necessary A-17

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: 4[gp.ftf D/EE. Sampie Source (check one): Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core jg,-/yfg7-lff:tS 4.,4 A ld /p:Gr~k Sample Location Description (attach diagram if necessary): loy/hdha/.seen% iAqA. a r t/m m le m hfo/ m af Me +i35 mm elevat%, 2elow Ap.rurface. Sag me<+ is f:, Hs a '/eff

  • ef cenkr/Ne, nex/ /a 4 2 O / 3 4, oceans 4

& nozz/e, me o(,Ga,. yeciness p ExaminatiorVrest

Purpose:

. D e % s,r e n a /se-e. Oi sne/al/S*c MW C* l'- f gases. Examination / Test Technique and Formatting: Afe/* ry47 ard SEM-5.DX, pfa fa o /.z3x m a' miuropr y As k 2Sbn SEM ages sad EDx ~y:m=.fra. essen /, a /A, jvs3.)dy/e fac( (See /ex/ Examination / Test Observation or Results: cr - Mefa/#cf(4aae wi%+ %bblek. Cers~<a '*s i.s Dre.s.e ~bu / er-esc 4 6,xNe' ) wiH 4/*e-ty/ed bi/s of o/ Zr-ss-/tdli' e/ Ae / f ases oud yat,6s/es a4 Cd ^4p th, Other Parent Breakoffs (Sample LoqNos.) and

Purpose:

  1. 2.4..D/E/ (me

~ 42d:> D /B.S (mef V sSEM), 424,.D/B4 Cm e /,.SF.?st 9-/?Ordness Comments: Add addilonal sheets if necessary A-18

s Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet i Sampie Log No.: .f2 6.D/.3.3 Sample Source (check one): Vessel steel dozzle Other (specify) -l Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core m-ar/n s z.A ** =<K

  • 'py*";

s m Sample Location Description (attach diagram if necessary): A' a yimeyr(e ni /soe al g' he M35 mm eA*vafrbLon ifudinaf Secr%; f4ro9 Ee/ou>y/se Ap Sur ace. l t 9 f l 59 rn e + is 4 He " rig 4 + of ceiderbe, ried*f fo 4 2 b D t.B /. O rr e ol' Aw yeesriets actoas /ap l itezz/e. Examination / Test

Purpose:

kfesm-ke ,,yfes,.e_ o,e meMb a s d w m s'c. p,s s. Examinationfrest Technique and Formatting: Mefaf re ce.d SEM- @X, y L lo m x. Maa<,pt, e/ 2.sx a d s. w e g s SEM />y and ED)< fra, re.x /g,/3) /e /*d'",, Examination / rest Observation or Results: (See Afefr& Asses are. essea dq cc-der (roo, s~e ?witA habbles a d s.me%d. Cr-nu ' /ek/e/s hekrogeneous fomerale \\ abse L temre" area s's a ef U-ro'c4 , 2r -rk j a A Cr -ric k. m nArix ca.s fsio,13 a ee a s0, M-an d n'- fue/ soAc/n4'ed' ist-sihr. Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

4 AZ:V3/(,~.es/ saa'S8'Mj 426 DiB2 (me H Sed., 426 2> tB4Grag Sswf., Aardaess.). I Comments: ) Add additional sheets if necessary A-19 1

Oate of Sheet Preparation: OECD TMI-2 Vesselinvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g gg6p/g Sample Source (check one): Vessel steel VNozzle ._Other (specify) Guide tube Companion Performing Organization: Principalinvestigator: Sample Core Grid Location: ,fAL-MCTl*fM L.4. AldNr72rrg f YS Sample Location Description (attach diagram if necessary): lbroug. aff X/ Ole #!flBAe-A fort //uebhal Sdncb' ors a/ Me vAss mm eleva&&n, bedw Q S u r fa c e, or, r%e 'Yef'/

  • SWe oY r/o2 Eld 2"l Jeparea f is mfanes ou Are.sur Aree.

Examination / Test

Purpose:

ky wsoe,s*se e n &lure-C'S "' dl//I'C 3**d' #~3"'k t k a.or d bardereSS of hde Arm er: f ases Examination / Test Technique and Formatting: /f$!do//gryAl SEkl.- E.D>C, a d 2>fX' "C'*A*'W"' - M actep 4i% paf.zsx,irricr y hoAn at 2rox. Examination / Test Observation or Results: ISee /ex/, yo, /J.) / ash 2 DfVI so/ af/Acc( h = !!1 elf usi/A 17ure,erens ffghr///c face. / cc-oscue ~ e ce. a,.,..-, ye,,.,,,, &//,.s ai, v/s fe' le /s.,.gom e a s den de'*le s.; 442r 'n

  • l'ix Ce -He A n eed'/e.*

liased uMH %1,1le

  • face Co, La devoid nent
  • "f<r is G--h***d AN4 ud I'/. Yerwc ' *$a of Fe, 6n,' Ag, f.l~riek 2n d Er~-rth h St<t l IA E!3*dc?

ice s, s

  1. 2 6.D/.S/6,se / >SEN1 Other Parent Brjakoffs (Sample > Log Nos.) and Puroose:4161)/B1 (mef F SEM > 4t6 DtB Comments:

Add additional sheets rf necessarf f A-20 =_--_-__ _-_--_ __- __-_ - _ -___ ______- -_-_-__ _ _-__________- _--_ _ ___-_ - __ _ ___

oV W N s Oste stigation Project Sheet my ve ar s lIn Sum e TMI-2 esation/ Test Other (specify) V OECDSample Examin dozzle Companion Sample Core ~23 Vesselsteel

  • 'yy ";

gyg3 Guidetube No.: r: PrincipalInvestigatoA. hl8/rn8/- SampleLog e k one): c Sample Source (ch l no22e / ry): dh9O K* ort Organization: diagramif necessaof Cast

  • l2M g

Performing p/,pfg7,/]'~ Description (attacsesf h /dete^' 70 '""" / 2-SampleLocation,y /o f / u h p1r %ce. / pu/er '"* h a [> / su / / d4 / w / He o/ ose:s k e dness. amination /TestPurp n har pe fe,,,,,u a i/s Ex iircfadig

  1. x' atting:

and Forms E?t4 E D X rop /s a chnique 4 Examination /TestTeAfela1 eaf y, a Xy V"'I# "# /ry'{C9 ic A sx, m fraa 9 af /s Macnp o/o s,ED b*# Au**d as l m )s's/SS,Mn Nl' B"d "'"* '.~ orResults:g 2%se e e An g a SEM Js/a Observation /S, /r gynla ly fa Fe 6* e. 7"y,oe M

  • "*4* o ~ 4lersl

'n' s e., f C fh Examination / Test 5 e e fur ra l>PH. N* a 2s />'s a w fece /s w/ ' s M 2

  • 6 'o x.t d e *

, unic a os wi cley s 2 /,7 ss 'of heav di ,so y4 A ;/oJ. rdn e se: fiere

4ujs gNos.) and Purpo ea ar islands,On e m(e fs /*koffs (Sample Lo b2

) gg//, y. 426 Other ParentBrea e or ne ets if n A/o al she n Add additio ents: m Com A-21

Date of Sheet Preparation: I OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: gyg D B Sample Source (cher:k one): Vessel steel 1-ffozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core gjyL-ggyl*ffS 4.8.hl8/or?B/~$ Sample Location Description (attach diagram if necessary): We/dne dl Castalb'9 on nozzle outes m y /ou.se:sf ~ 7s ~~ e / eve h n. su, pace. af .1hr /ermore na be o/ fAe &*.he d /!e-l m 3 N'l3 { Examination / Test

Purpose:

inc/udig ;/s A, dnesg. Examination / Test Technique and Formatting: AfefaW raf y, SEM-EDX. A NB af SSX, m /crophe,t,, 4 sooox, .Sf* q olo f Ars mye s, EDX y A-a a Examination / Test Observation or Results: h*' Va!I*u5 "cer**/c

  • I Acce

/s. Ir9u Iaely.s/ssyned' *=*d

  • h furfaees. 2%pse mer's/ /s /rylCr;,

cleps/As oe /o *% A/i, 72 W/ Fe. &c. 7 , M,y Aund as ista d. Macs,,e,s is in u 5" u. to4 SSAre)y ~to 5 Fe -Ith//* No = k "'= '= 4 of heryv *oxtde

  • we s 2 s Ce ~

meklo One area }{e/s//ogra;pdy :sdou)s f/rrefy disyVrsed, uitt'deot/iA**dfg*hf'06 V v Other Parent Bre'akotts (Sample Log Nos.) and

Purpose:

hl0n e 42 6 'l>2 e or Comments: Add additional sheets if necessary A-21

. ~. _. - - ~... _ _ Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: AM. f26.DSA Sample Source (check one): Vessel steel V ozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core Gr tion: jj ggggg Sample Location Description (attach diagram if necessary): elevak of JAe. ~7~ransvetse. Set::libst. a f hie-O mm t M5frumes / cen ht-of nozzle. Cap ures masf o/ f .5"rl'*Ce l"'8

  • SbM t

pre /y, segm os1 of noeafe. innes~anr>u /us, kd som, e. gae/ oZbc. delv<lg My/ in der Nh lt del 9t'Is be/wees lyf a*ed stk%EZle Examination / Test

Purpose:

in / /At I" %n,he e nsfure ef noefe/4*c Me m o /* /A'c.sheeds?<% %e /* ' * * ~

  • f Mg"*annu fu.s,He me/m/heryca/.sto/e. a/ Me h s /ru m en +

1 And seines;, Examinationfrest Technique and Formatting: aa d Seef-EDK Afef-fyre ya/25X,srt/etwfofus d N A50X* Afactafrlo

poee/re.

SEM images ad e%* Examination / Test Observation or Results: h ef d** yon /Nos I.s 72 Wall-WR-/4 TAe deisris in Mt p B"ufu s of Cr*Ne' arfr4Yes v/M U-2r imjourM'e s.onsi.s/s> c 7~h e.sAards (on aler-hahseen for s/eu m a. 4 a ee. Znc. Goo.+ Q, _,,,,)is.,+~ a., / /eeds ore /ea/s be dr*** S **/ / cracke.d, edlfle eHen m ay 7ad?a/;d;' pleelos c< -e., ise/ sufficien//y diftadhve a f **ros

uekn, Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

424.D38/ 68e/ 426 D3C / Gne/, Sept a~d Aardc<=s) ~ Comments: Add additional sheets if necessary A-22

= _. - Cate of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: A gf 333/ Sample Source (check one): Vessel steel IATozzle Other (specify) Guide tube Companion j Performing Organization: PrincipalInvestigator: Sample Core Gr ocation: yz, yc7.,. /yp3 , g, gg,y yk Sample Location Description (attach diagram if necessary): ~7~rans vers e sec.&o,t % M< ou Aer wrface =f Ae e/evak, Cay /uns

      • j nozz/c af /he o mm of He surfree, syon /

e ~ t.r m m Examination / Test

Purpose:

3lruc be

  • b bb'

,5 t~3Ist I GXa***i% e flr e. /s Amed, ass. and de%,ye l l Examinationfrest Technique and Formatting:/ measurem u /s. }{efs//ogrejoAY anc( '2>>94 Le /os a/ ux Gnelehed' ~ d e /c led).,mtenykok Mac 3b 'CX *.*DPN measuremis. Examinationfrest Observation or Results: Mittos/ruedure, /Au./ o A Weldorenf, illeN fesses &*d cas/ sfruelta-e eviden C b d**ess is .a ri.t/3.D P H, Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

42C:,D3,4 Greut sad SEM)., 42 6.2>.5C/ Cme 4SEM, Aa"4***s) Comments: Add additional sheets if r:ecessary A-23

Oate of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet i Aj!$ fff336/ Sample Log No.: Sample Source (check one): Vessel steel VNozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core ,4M:.-Mer/.rps A.,4 A/e/ mark

  • 'hj " ";

Sample Location Description (attach diagram if necessary): &Bossverse Set.fr'q hm /Ae ou led-Surl ace ob ASC h Cay uns oz2 /e a/ +Ae es mm e/evako. of dy/4 insuard, 425 m m of Surface an d' ~somm Examination / Test

Purpose:

d es//s examne Me Zac. 6 oo Eva/uale a s / y qrair.skack, ce,ue see e/e.fes m,,x ene /,a,dnesg, an d Examination / Test Technique and Formatting: N<'./e//sprayL, SEM-EDX, and '1>M measumenis. Nekrof o+o u,e k Aec() Dl 9.6 kj f'?lC'#faf chh 2l A /oo and /.COX) bardness m easter ca w f.s in hPY, Examination / Test Observation or Results: /992 P2>PN (ayg et.5 mess.) .s/ rue /gre of yao* 9xed faIns Won-4<=s<;4*/yyym gra;;t uf

s. g m,,, in diame /er.

Sme Me= Nag lrri n.s of.seen d ghoses f/WSen f. & pre,, f precy;fa Go nb* YB r*S DA b., u)I HsIn gr ains an d a4 gt ain sef,e a la er. mixhee */ he e*r* a'ek.s sop. -Hter o,eis'a par Neles a4p oxid'e. Cxthe 5 pars ib he Fe-based'hol ana p Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

42O34 (me/ Y SEMX 426 D3B/(trie / 9-Aerbess) Comments: Add additional sheets if necessary A-24

i l Date of Sheet Preparation: / [2. - OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet l Sample Log No. gg/g/ Sample Source (check one): Vesset steel dzzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core Qf-jfg fg /,4, A 6lrn SrE ' h)'f " Sample Location Description (attach diagram if necessary): g. L'erngik din a / Sec Ab 1 O r # "i) jn 6 sf no 22.le daf ur-e.s f me hin.c l Sbar s and hel fraagmeds ,h a fiae fBrficula fe m afr-Ix and orie. sic /e c,.f i \\ y ilozz /e-innen.s urfa c e. i Examination / Test

Purpose:

De.fer' min & A & bu rC $Y $ b riS c2nd 01 e_ parfica/ut-e. <nateix. 1

f. 7 fg,N Examinationfrest Technique and Formatting:

N 8 /p//o r A o%cl $$~ON* ua x-ray speche. gg,y e, Examination / Test Observation or Results: very Ane (</co,A)as.fue/ a{echPorf cle s M be/ Afafiix is o p wyin c-,,s s wo, c compost hon s, e. 23 9l -ir,(ze., Sne ceibzed are usetous ib. fe mosh ples % l eiec e ,f .c Fain i esa con %ae-ea,,.a fis e., + of m, A-ix besides u asa2c. Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

af EIBz (met, SE/v/ and hardne's Comments: Add additional sheets if necessary A-25

Date of Sheet Preparation: // A p OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.

  1. & E/BZ Sample Source (check one):

_ Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core hl~/ lL'ffff.6 / A

  • W&l7?S$

jj Sarnple Location Description (attach diagram if necessary): 'h b.0/>sibuobbD/ $6cl/d4 en /1032/6 ktf inner &d ou &.carfac.es. Examination / Test

Purpose:

.Ddsemine n aface of stoz2le degraefafibr. 'De fermi <,e / paral,ess. Examinationfrest Technique and Formatting: YC 7'B//q , $5Nl~EDX, tr1ECrob Br$ ness. Opi6;co/ p 43, SEM Dnageg, x-ray sy fro, s e d b w w tu e s. Examination / Test Observation or Resuits: k/ /7?&lor $HPface, V8Sc./c%s/. 04 kr' SWrf2L6 Close 24 oe ep/ so/;*cks feqrefure. Ou/er-Ael {fPeal + Aa f lea .s ueface.sk ed ' micro - 4/c/s , 2rbicle c, no a Ner inch DIM p&r ficg/g {c g NBrble 5 s is 2026.291>PM (avg. of 7 trd as w m /s) -#26 E/A / (m' esOther Parent Breakoffs (Sample Log Nos.) an us srg Comments: Add additional sheets if necessary i A-26 l

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examinationfrest Summary Sheet Sample Log No.: 4

  1. 24 EM/

Sample Source (check one): Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core 4m.-m7yr' s::'s L. A A'eimarAC h l)" "* Sample Location Description (attach diagram if necessary): 'O'ansversen secfor of nozzfe Mner surfane S q M nt-f 8/ Hre 274 mm e/evar6*en. Cyfare.s me/*At t'an deren on inner.s u r / a' c e and s ~ ~ e p e l/cu /a f e Ceramte elebr/s aleng in n er-s urd' ce, a 1 Examination / Test

Purpose:

J'>e i ermtro e n a/se-e o/ m e la///c twndron an d par /rc/es, dhe c es emre. d8h/ec dozz /e h ar c/,,e s s., l Examination / Test Technique and Formatting: Me/* //*gcap,9 aa& SEM-EDX; TV// measumeds, Nfacrofher a f 9.le>cj SEk/ insages. ekd KDX t.a, Examination / Test Observation or Results: i Ma///e runcleum e-arh;gaeus wi+k base metal ad coactudad,G, be hC* W $0$15f3 )Dh"{ernndNWh$no%peyg & g r g /g & g g ueri of fuet s4=eds, fuel 1,e in an re-6,xs) fut letx (i/aerat,.y w a g o,,,erate st,rs)tteles vieldhr sl a,a exi,,,,,,a, e.aWih.,is, e.g. c,, su.,n/

  • W en

.,o core m 3 enafe,/ red cea eds ist U/dr r et%s fre-e.oz le n. n twoc.h'n*areareas oa Zee. s u o-ec, l, EM s po/g4for-bre /x, 4/ and n rh/3714 DPJJ /"avs. e/ 9 measueemde e .m util r; ee s,s is Other Parent Breakoffs (Sample Log Nos.) and i)urp"ose: 4,2d> E244(SEM @*a' Aetdeess) i Comments: i Add additional sheets if necessary I A-27 1 l

W Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: AM pfgf Sampie Source (check one): Vessel steel dozzle Other (specify) _ Guide tube Companion Performing Organization: Principal Investigator: Sample Core ,4 M. ~ / V/ c r /.Z % f,.,4. A/e.imat-K j',*# Sample Location Description (attach diagram if necessary): op ito2z/e o u fer.saeface ~7~ransverse. seei Ses me< + af +4 e 271 mm e/evakon. Cefuns

  • 2omm o f oufer
sueface, Examination / Test

Purpose:

"!##bb"S 1)e ferm/sr c nBlure o S Dy 5"'l*CC

deposifs, et-De fermin e izozz./e hardneSc Examination / Test Technique and Formatting:

//e/arYy/ A R.ed.S~Ekf-E.D)<,* pf;/ measurem en.fs, Macroeod-a K a/ e.sx; seu i,,,nes o a avx Sfec /ta. Examinationfrest Observation or Results: (Tee /e.x/,p.21.) f l l defss//.'o -2o,C,9 7y % H,e ZKconef.Ged

u. z!A/c 4'. f f o S /ayers Nu///

ens / aue/a' ce /ayer:s c:ew fant peineya//q /aden Znner-Fe -etc fu arr9' w/ / k,4f 2,. y,,g' .Q Oule+ /ayers an [eae.fe d' reg /cn Con iain ed Cd,In, s4,,4/, gr, Si in add'/liost g fo en/ranceef Fe an d Cr. Rese.fran M/er k MXDM ko 54Pd"%%%"V% Asbe,pranatae Ch* una ew. r Other Parent Breakoffs (Sample Log Nos.) ahd Purgose: 4'24E2,4/ [ TEM sad /radess) Comments: Add add;tional sheets if ne:essary A-28 L______.______________________._

i l Date of sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet i Sample Log No.: 4 h gff Q Bf Sample Source (check one): Vessel steel FNozzle Other (specify) Guide tube Companion l Performing Organization: PrincipalInvestigator: Sample Core 4NL-Mer/ZPS L >4 N'4"" A

  • }' ' j'*";

i Sample Location Description (attach diagram if necessary): "T~r~astSverse Set:/for o/ noazle oufee sudace oI

  • / '"W'M a /S mm t/se 90 mm elevafran. Capfures and ~/o mm iotl0 sto a t l ej a b ee / S

.f,zg g.qyg, i Examination / Test

Purpose:

~DeNhe /n e n afuce of surfac.e deps/h., Deferrnierc. it ozz le // R r/ess,, Examination / rest Technique and Formatting: f P. 6 y; m/et f, 3A6' "'en urm e<.s, /t/gfyf/o A S E &f -di'D X les af/50 Ad ShW, pfgero la SEM /aiages and SDx -yeefra, i Examination / Test Observation or Results: Novgadfer ed 0./3,mm J/s /ck SColA on 3urface. Gn tafx.c s4we As aor Fe.rtel m a fr/x,, p fp ueer e/ par //eu/sle addered /w er d-za-A a f. s o,u. SAdea's are peinerparty no2zle

  • Fe besec/. /-s,t4 parfie /es
  • Asp /A' y/*yer ort As -cb; 1'eaees a,c are z,s,

/9oL / *7 Z>P// (Qvq. of 8 oncasaremesfs wdh E-4Bh i $3r'dna ss i:s, Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

426E4B.B Gyardness) Comments: Add additional sheets if necessarf A-29 I I w

Date of Sheet Preparation: OECD TMI-2 Vesselinvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: A[g.f264~gE3 Sample Source (check one): Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core Grid Location

  • A NL - M d f lJ M~

L. A W 8 N !? W $ ff/ Sample Location Description (attach diagram if necessary): -n assverse.seedent af naaste innee-sueAce al Me 90 mrw elever9er. Cydures a/S met af surface kd ~/s mm info noez/s; RAu/s 42s 14.8/. Examination / Test

Purpose:

M!ne/ne sta/nere o$ Gnj surfase Wy* sib, .Dc f&mthe /fo zz/c

kBdMesS, Examination / Test Technique and Formatting:

Ud'7'alqra,ead SEM-EDx, a,,d 2>PN harda' ess Macnfofo e l F. l> X. SEM exam stof ferlormecf o Examination / Test Observation or Results: hkees /:s /90 f/92NW (Mg. *f f "'**'"***S Wo'fA E4J!i'/), Other Parent Breakoffs (Sample Log Nos.) and Pu ose: -h6MB/ @EM en d "he". Comments: } Add additional sheets if necessary A-r30

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project t Sample Examination / Test Summary Sheet Sample Log No.: Ah gfff$B Sample Source (check one): Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core Aa.-acr/r/ss L.,4. A/ennart

  • y**""

Sample Location Description (attach diagram if necessary): Tr'ansverG e Sec./7'or of boWom SurbCe (77 m m elevafro>,} of removeel s'tiskume't f .s/Hng Q 4 Examination / Test

Purpose:

Delerm!na nalure ef exfraneous m a W ia(s. Examination / Test Technique and Formatting: A es x ; SEM-EDx no+ ergrated. Mefaro Ysojco ces/er du be. M lo s MQ }o /cooy, Examination / Test Observation or Resuits: Meb//it.. shards Arsve een fer /ube a d be&n // anaf in 5 hum en. / /e a d.S 9 eGr h be-W some sw faces beiHte frae fuees, bu.f roue dt% or supes f c/uc&/tg ae-.sh/ p%d 4 L leuf, era (wes. Possibly cuJh'9 debris Trom no22 e. a q ui ikon. ~ Other Parent BIeakoffs (Sample Log Nos.) and

Purpose:

YOM2. Comments: Add additional sheets if necessarf A-31

Oate of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet 4 486 [// 2 / Sample Log No.: / Sample Source (check one): Vessel steel t 14'ozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core Gr Location: j, g,. ,,g Sample Location Description (anach diagram if necessary): Longthe dirva i sec+io n of nozzle ir7r>er sc<rfac e "/ # af /Ae +o (< 2 9o mm eleva6&. Cyk'*es ,$icle of /s) e/.Setrface. of~tto22le, i'ISN""*" son 4i,epac+;of),ad 4,s n es+ ss % re-"= 's. of ma/eria/ ("me/s/l$'c) ube/ueen Examination / Test

Purpose:

i kferirr/,, e, tya r ui~e cernse %s/en,fg, a /(sza /e wd cow das f; 4 ar'ure-or bad dafut e-ef gr.np lij uid'- oferr/ lase., Examination / Test Technique and Formatting: Sctt/-5DX, efv., da f e6x, intykfos si'L6OL /We/afog/o 3" "'"VS placropGDX Nd .S ec /r-8, Examinationfrest Observation or Results: 74AG-/Kr-Afe/WJc fase in amou./t< s i.s e.scea//a/fy Inc.Soo base is afsa Inc. rf,M*-/SCr~ // ?"))* S eIL G'. JVoz2/e ilex/ fo abo s'e (XI*Ie Co*du} / en In c, hemsc, * /s C# -o. OA fur-faces, 4f.,y/ p.,;e g ses ;m, fitc, noaz fe, yo.,oo,,e4 5,,, &e/ Cl~2r) Shaeals fre he foiefs or# So //c/ M J e d' e/e/ i.s Ce@xide) en ' - u,-dghose. af lof ofnezz.fe, Gra s%fds en sfain fesg a,du7( Other Parent Breakoffs (Sample Log Nos.) and Purpoee: & f/AW (Afe d SEA'h ABAC+3 Comments: Add additional sheets if necessary A-32

Date of Sheet Preparation: f [2.- OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: g g g [/ g' [ Sample Source (check one): Vessel steel gNozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core k/V/,(([ fg 4. A. W a k es d $)$# Sample Location Description (attach diagram if necessary): 0A /?0DlC LCng/kdina / Sec$0n, Sf /J mir) slousi% hy wd sid'e sac faces. fSc.< b s Yhtfe kr 426 f/ A/h Examination / Test

Purpose:

D9.lerm s'n c A a lu l'~e 'Gotd ex fest l 0l ? . car-fa c.e idera c.}iort. l Examination / Test Technique and Formatting:

  1. }?/a//of CEM-E2,)X, inicb& ness, Opha/ >yk hist p6gs 5 x-ry sphs,

~d Examination / rest Observation or Resuits: l Surface oxidk % of de a,rd 'n - w e U involvemen t A / pene Aro7%n beneuf/ t DXId'e areasjn/p at% fM5%< f Ap <d wiM W W Nat l ff-2r tiedu le:, k Soap Ave, h ardnesswf(0 = mom.DPhi i Other ParTnt Breakoffs (Sample Log Nos.) and

Purpose:

Y0k fM6/$9Yogr y M N.9 f/ l-6 W Comments: Add additional sheets if necessary A-33 i t-

Date of Sheet Preparation: .4//h 2, OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: fff gy/ Sample Source (check one); Vessel steel XNozzle Other (specifV) Guide tube Companion Performing Organization: Principal Investigator: Sample Core Grid Location: k/Vl~ A'l$7~ W& )s k iY8N?2 2P'k h /Q Sample Location Description (attach diagram if necessary): frai>s versa se as, a f iso 22 /e surface a/ Me 266imt elevaken. Examinationfrest

Purpose:

Defermh e. /ta/are of sueface debris w& O22/e degradaSon. Examination / Test Technique and Formatting: Me fa//ogra , SEM -EDX, ancl *Icrob&"cl*S i GEAf ;P ol09re'f S1 N Po] T h N O fica / as d f Examination / Test Observation or Results: f,c.e a b /> h u h 2mm deef>, I"regu/*'/Y ** p,f e c e., 4,,;.s s,;,p 4/ pene fraflon, cc + ri sadace sur-e oxlela k r 0fveclaict eik Fe -oxide Cdb M /ajers /J-2r/A - Cd 7'*rli c les ~ kr innee '~ 9 Fe-rich I*aye;r. Averap e h ardnecs (s') VM1>PM Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

Yf//d Comments: Add additional sheets if necessary A-34 l 1L___

aw..a e-k Date of Sheet Preparation: [/ 2-OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.:,4 gggg Sample Source (check one): Vessel steel t /f6ozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core

4AH-Mcr/Tr 5 L.,4sk/ mark
  • $f; "'

6 Sample Location Description (attach diagram if necessary): S pin e is a fransverse_ C/*oss -seedbn o f fle-in s eu m e,, f a/rin 9 af /Ae /58 'nm elevakom Examination / Test

Purpose:

De.fennt,,e /Ae n a fure of Conduif b rdabor inablal ine./ //urgy s f s'-Q IttSide Cofe,osed fuje, wd He re-had ast res,, I Fr.mination/ rest Technique and Formatting: A 7 chgr q s,. M a at/ogry by a,,d sEM-Ebx. Op Rea/ SGM irnyes ad x-ry pFra. Examination / Test Observation or Results:

  • Ybf eXc'dI2elj ^Cr-clep eM

$~l Bin less $ bent / dew dt<.1/ kBS ik khe i.s l reac /a.f fs L A d. Ma fee;a/ hage ha d' '*CSX rdEC W .TnCone{, En V) ires generafly b"n d* $'?d W I r t u>o'fh. Al2.0 IAsula fiosy 2r -A/ Su fee-lic a B ea me.(hed 2isd llsen reae.+ed tejlN Cone l 3 Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

n/0/7e Comments: l l Add additional sheets if necessary A-35 l

Dato cf Sheet Preparation: 2 4/,2.,, OECD TMI-2 VesselInvestigation Project Sample Examinationfrest Summary Sheet Sample Log No.: g[g Sample Source (check one): _ Vessel steel MNozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core Grid Location: kNL-NCT/IM L A WeimarK T) /O Sample Location Description (attach diagram if necessary): 77 anwers see % a+ no2zle surface af Me /.68mn? elevskon. Area is of gross, %fergraasdar ' ca vi +i es TA /zozz/e, Examination / Test

Purpose:

1)efermi<> e nafu ee. u d cen d * / (- Gvi Ne s, and miceas.few+uce ef no22/e. Examination / Test Technique and Formatting: ge/Bll}rf, $d0bi-G'DX,.%cL microhardness, f h A Cy ce/ cn SEM f oloyaf sj x-ray Wre< Examination / Test Observation or Results: Cat;/.ies .f!//ed wi/L fu e / clebris ir 6--rich 'n a fr1>c. A -Cc/ Inner Su daeas h ave Cr-6xide) /syet; g .chluerz in grain bean deries aref a s srnoll eak micro inukm flodaks in. norrle enafrix. Largeuna/% +w.s s,p'and tua h a<d.,ed s shve d gre, ins 6 24 3>PI-r) IndezRve o f hh,L 4euernkre. ~ f;%M]$ (renkel Inc, nagg and F406?x'NI#' Nkg Other Parent Breakoffs (Sample Log Nos.) and Purp e: Comments: Add additional sheets if necessary A-36

Date of Sheet Preparation: / f2,, OECD TMI-2 VesselInvestigation Project Sample Examinationfrest Summary Sheet Sample Log No. Qf[g Sample Source (check one): Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: Principal Investigator: Sample Core ggf' -Q[fl7& / 4 /1 /6's E & I~ $ Sample Location Description (attach diagram if necessary): 9 /g j$ fr on c en fer of 4022lE 'D E lbO Inff\\ g/g fly, &ga .5 bo u)S Ft022l t S"O MS 'E 79 + +r ge.s t~ a m h. Examination / Test

Purpose:

gfemx /) a kc,_ of /Agof and see.K e vi den e e. 4;,,r-raase,r 4r-mahria { Ioss o~ n ozzle TD. Examination / rest Technique and Formatting: $6*/ f-OX e bW f fJ j //fefal/opryk ~/ CEnl images and X-r ~qec2ra. Examinationfrest Observation or Results: 3 p ;, c,.. J /mg zuenel wifL Cr-oxhhu as We6 e+ sac h ee. 4-cd nodwles ir %ofs Fe-rcet a re ag pr&aWy o Aides. ID o# a3 m u) i= o~ D ito12(e dehe;ed in Cr$wMcLo /]h. 2 Sarl@ce Cd&M pth&ce_ kew /qrolokW a s. eJem e.6 o Her M es C r,7"i, 4el Alo,- sgsi ttp Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

4% F4A, 4% F4C. Comments: Add additional sheets if necessary A-37

[ji9k Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examination / Test Summary Sheet Sample Log No.: f/ff'"gC Sample Source (check one): Vessel steel Mozzle Other (specify) Guide tube Companion Performing Organization: PrincipalInvestigator: Sample Core G Location: gg_gg gg. g Sample Location Description (attach diagram if necessary): f /C is bMM 5" area 7P signiRco.d dabiis depi/:or /c8mm ake k & ~ d nozzle. debn3 f h Examination / Test

Purpose:

DOWilis e nalt< x of S*H WGce -Mer,$a/ y aepfes in ferac.+im uML no 22le, y el ir He no 2z.te. Examination / Test Technique and Formatting: k sEM-EDX. MeJanograpj y, BynIf(caNor NQ/t k d bid in s G goliskec[ ofc8 l senge 19 PGfoyapx s. H L aul lous egnuna{m h 4 and rav 5each-a, Examination / Test Obser)lation o[ Results: a feu) hel d Cr and Fe ox; des,Inconel neM. Debriz is a migtw e ar+(ch s asa russes J Ce-Q letect p' blo221e bueface

  • Merack invo %ed Cr oxiclafios ad

-Gv.nd in kl penebra+iop. A - Ccl packetec g n.o 2 zl e. and ix Cc-elepleled <nasse s. Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

426 FA A, A 2.lo F4B ; s w e-9 arpose, Comments: Add additional sheets if necessarf A-38

f cate of Sneet Preparation: /o /4 92 - OECD TMI-2 VesselInvestigation PrcJect Samp'e Examination / Test Summary Sheet Sample Log No.: ffdI((A M [ Sample Source (check one): Vessel steel _(Nozzle Other (specify) Guide tube Companion l Performing Organization: PrincipalInvestigator: Sample Core &L stfCfffk /, k, YG/k W$ Sample Location Desedption (attach diagram if necessary): g,fg j, (m, /A e. r2ozzle S ex r-fac e Gl YG $2 ryfr) 6/6/4 fl* " - l Examination / Test

Purpose:

behermin e tra h r-e Oh lUf*f Sunfac.e. l Examination / Test Technique and Formatting: 0 I'E3l

  • f

/1//e}D//egr 4 $$ ~.DX

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ggM (m ages, nn el K-raf s f iwic,,s .-J., m Examination / Test Observation or Results: 56x) ma4-ix codaiss fu e / s4s,-ds a f Va&H^ ev? awl hi4 naale. surlage fremad compsi//en s. Dt layers wiM A/Q A4].Tn, //M/j.,4 a,,d Cd h <ct la fec5x) byer Other Parent Breakoffs (Sample Log Nos.) and

Purpose:

i4de/~/~9 DI';I #l gg fg fyr{cTae Comments: Add additional sheets if necessary A-39

Date of Sheet Preparation: OECD TMI-2 VesselInvestigation Project Sample Examinationfrest Sumr,try Sheet Sample Log No.: g ggpg/ Sample Source (check one): Vessel steel dozzle Other (specify) Guide tube Companion Performing Organization: Principalinvestigator: Sample Core Grid Locat!on: Am.-Mcr/rps L. A. NeimatK 2)io Sar.,sie Location Description (attach diagram if necessary): -n ansverse sech k o f ou /ec n o z 2 te. s uefue af Me 69 mm e/evakn. Cap /c/ures 9 5,,,,, 0 secr/nce and N 7 m ik& dozt m Examination / Test

Purpose:

kle %hre A a here-o$ BM S 4'rl ace. l Eye:r$, i Examinationfrest Technique and Formatting: Afefa// ry }nr d <$5H'-EDX. 3>P// hare / ness,. / W a c r o 4.e a f 6x. MM insages ad DX Examination / Test Observation or Resulth.gg g 75ie / of vndable He' chess, / k, tdo. Layer %s ' in s,- e p/~ esi s ~ <s .s d,- a a-r L,, d usere Af S, A, Cd,Zn ad p /e - A s ca., faned uj ze,gMo in A4/ des / eu/*r bsa ds a/sa repV n of lvver, Other Parent Breakoffs[ Sample Log Nos.) and

Purpose:

YOM2 Comments: Add additional sheets if necessary A-40

Distribution for NUREG/CR-6185 (ANIc94/51 Internal: L. A. Neimark (15) P. Drucker C. E. Till R. W. Weeks R. B. Poeppel W. J. Shack D. R. Diercks T. F. Kassner B. W. Spencer TIS File External: l NRC, for distribution per R1, R3 Manager, Chicago Operations Office, DOE ANL Libraries ANI-E ANIeW Manager, Chicago Field Office, DOE Energy Technology Division Review Committee: H. K. Birnbaum, University of Illinois, Urbana R. C. Buchanan, University of Cincinnati, Cincinnati, OH M. S. Dresselhaus, Massachusetts Institute of Technology, Cambridge, MA B. G. Jones, University of Illinois, Urbana C.-Y. Li, Cornell University, Ithaca, NY S.-N. Liu, Fremont, CA R. E. Smith, SciTech, Inc., Morrisville, NC D. W. Akers, Idaho National Engineering Laboratory, EG&G Idaho, Inc., Idaho Falls, ID C. Alexander, Battelle Columbus Laboratory, Columbus, OH S. F. Armour, USDOE, Idaho Field Office, Idaho Falls, ID l R. J. Barrett, U.S. Nuclear Regulatory Commission, Washington, DC l E. S. Beckjord, U.S. Nuclear Regulatory Commission, Washington, DC l S. A. Chavez, Idaho National Engineering Laboratory EG&G Idaho, Inc., Idaho Falls. II) l N. Cole, MPR Associates. Vrashington, DC A. Drozd, U.S. Nuclear Regulatory Commission, Washington, DC R. O. Gauntt, Sandia National Laboratory, Albuquerque, NM S. Hodge, Oak Ridge National Laboratory, Oak Ridge, TN M. D. Houston, U.S. Nuclear Regulatory Commission Washington, DC T. L. King. U.S. Nuclear Regulatory Com r.ission, Washington, DC G. E. Korth, Idaho National Engineering Laboratory, EG&G Idaho, Inc., Idaho Falls, ID R. Long, General Republic Utilities Nuclear Corp., Parsippany, NJ i

M. Merilo, EPRI, Palo Alto, CA R. L. Palla, Jr., U.S. Nuclear Regulatory Commission, Washington, DC M. M. Pilch, Sandia National Laboratory, Albuquerque, NM J. R. Rashid, Anatech Research Corp., San Diego, CA K. O. Rell, Sandia National Laboratory Albuquerque, NM J. L. Rempe, Idaho National Engineering Laboratory, EG&G Idaho, Inc., Idaho Falls, ID A. M. Rubin, U.S. Nuclear Regulatory Commission, Washington, DC R. Schmidt, Sandia National Laboratory, Albuquerque, NM C. Z. Serpan, U.S. Nuclear Regulatory Commission Washington, DC S. P. Snow, Idaho National Engineering Laboratory, EG&G Idaho, Inc., Idaho Falls, ID T. P. Spels, U.S. Nuclear Regulatory Cornmission, Washington, DC L. A. Stickler, Idaho National Engineering Laboratory, EG&G Idaho, Inc., Idaho Fall.s, ID J. Sugimoto, JAERI. Tokyo, Japan G. L. Thinnes, Idaho National Engineering Laboratory, EG&G Idaho, Inc., Idaho Falls, ID S. Thompson, Sandia National Laboratory, Albuquerque, NM J. Tulenko, U. of Florida, Gainesville, FL U. S. NRC, Div. Technical Information & Document Control, Bethesda, MD K. Washington, Sandia National laboratory, Albuquerque, NM R. J. Witt, Dept. of Nuclear Engineering, U. of Wisconsin, Madison, WI R. W. Wright, U.S. Nuclear Regulatory Commission Washington, DC J. R. Wolf, Idaho National Engineering Laboratory, EG&G Idaho, Inc., Idaho Falls, ID l l l

NRC FORM 335 U. S. NUCLEAR REGULATORY COMMISSION

1. REPORT NUMDER (2-89)

(Assigned by NRC. Adi Vol., Supp., Rev., $2T03E BIBLIOGRAPHIC DATA SHEET NUREG/CR-6185 (see matructsns on ene reverse) gyg,9475

2. TITLE AND SUBTITLE TMIV(93)ALOl TMI-2 Instrument Nozzle Examinations at Argonne National Laboratoly 3.

DATE REPORT PUBLISHED MONTH l YEAR March 1994 February 1991 - June 1993

4. nN OR GRANT NuuoER A2220
5. C.UTHOR(S)
6. TYPE OF REPORT L. A. Neimark., T. L. Shearer, A. Purohlt, and A. G. Hins Technical
7. PERIOD COVERED (InckssNe Dates)
8. PERFORMING ORGANIZATION - NAME AND ADDRESS (11NRC, provide DMsion. Otlke or Region, U.S. Nudear Regulatory Commissbon, and malling aMess; R contractor, provUe name and mailbg a&fress.)

Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439

9. SPONSORING ORGANIZATlON - NAME AND ADDRESS (11NRC, type 'Same as above"; Rcontractor, provide NRC DMsion, OWee or Region, U.S. Nudear Regulatory Commission, and mening adess.)

Division of Systems Research Office of Nuclear Regulatory Research U.S. Nuclear Regulatory Commission Washington, DC 20555-0001

10. SUPPLEMENTARY NOTES
11. ABSTRACT (200wordsorless)

Six of the 14 instrument-penetration-tube nonles removed from the lower head of TMI-2 were examined to identify damage mechanisms, provide insight to the fuel relocation scenario, and provide input data to the margin-to-fathtre anal. ysis. Visual inspection, gamma scanning, metallography, microhardness measurements, and scanning electron microscopy were used to obtain the desired information. The results showed varying degrees of damage to the lower head nonles, from -50% melt-off to no damage at all to near-neighbor nonles. The elevations of nonle damage suggested that the lower elevations (near the lower head) were protected from molten fuel, apparently by an insulating layer of fuel debris. "Ihe pattern of nonle damage was consistent with fuel movement toward the hot 4 pot location identified in the vessel wall. Evidence was found for the existence of a significant quanuty of control assembly debris on the lower I cad before the mas-sive relocation of fuel occurred.

12. KEY WORDS/DESCRIPTORS (List wortis orphrases that wi# assist tv, searchers M Jocating ins report.)
13. AVAILABILITY STATEMENT TMI-2 Unlimited Instrument nozzle
14. SECURITY CLASSIFICATION Fuel debris crusts frNs rage; Inconel 600 Unclassifled Fuel debris relocation fru, Raport)

Molten debris interactions Unclassified

15. NUMBER OF PAGES
16. PRICE NRO FORM 335 (2-09) m.

I Printed on recycled paper Feceral Recycling Program

UMITED STATES secc1At rounm ctAss RATE BUCLEAR REGULATORY COMMISSION POSTAGE AND FEES PAC WASHINGTON, D.C. 20555-0001 usnac PERMtT NO. G 67 OFFICIAL BUSINESS PENALTY FOR PRIVATE USE, $300 C' 3+ it-1911

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