ML20083L847
| ML20083L847 | |
| Person / Time | |
|---|---|
| Site: | Crane  |
| Issue date: | 10/27/1982 |
| From: | Mccracken C Office of Nuclear Reactor Regulation |
| To: | Benaroya V Office of Nuclear Reactor Regulation |
| Shared Package | |
| ML20079G498 | List:
|
| References | |
| FOIA-83-243, FOIA-83-A-18 NUDOCS 8211090598 | |
| Download: ML20083L847 (1) | |
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9 Jd. Q OCT 2 7 882 MEMORANDUM FOR:
Victor Benaroya, Chief 34C Chemical Engineering Branch
.4 Division of Engineering
{C' FROM:
Conrad McCracken, Section Leader Chemical Engineering Branch Division of Engineering
SUBJECT:
TMI #1. 5.G. CORROSION / REPAIR EXAMINATION OF REMOVED TUBES Enclosed is the Battelle, Columbus final report on failure analysis of tubes removed from the TMI-1 steam generators.
This report supplements the results of the 54W report which I distributed on August 19, 1962.
In addition, reports on the RWS retainer examin-ation (dated, May 20,1982) are being distributed for staff review.
These reports, along with the previous ones that have been trans-mitted to you will be referenced in GPUN's safety analysis, which we expect to receive by the third week of November.
We did not receive enough copies of these reports for a complete distribution.
Acopyofeachreportwillbeavailab1pinmyoffice.
h L
Conrad McCracken, Section Leader Chemical Engineering Branch Division of Engineering
Enclosure:
As stated cc: w/ enclosure POR 50-289 R. 01111on cc: w/o enclosure R. Vollmer E. Murphy D. Eisenhut P. Grant W. Johnston P. Wu T. Novak
- 5. Young G. Lainas R. Jacobs J. 5t'1z L. Frank S. Pawlick W. Seagraves, FRC T. Sullivan Dr. MacDonald, Ohio State H. Conrad J. Weeks, BNL W. Hazelton C. Dodd, ORNL J. Rajan L. Frank DE/CNE8 DE/CMEB CMcCiic'2 ken:ao VBenaroya 10/
/82 10/ O /82 XA Copy Has Been nt to PDR
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Form LRC-139 (l$
Research and Development Division LYNCHBURG RESEARCH CENTER Babcock &W11cox tYNCH uRo, momix IG J. E. MATHESON, FUEL ENGINEERING, NPGD
[**((}ER From 9.ADIATED MATERIALS TECHNOLOGY, LRC Cust.
File No.
GPUN or Ref. RDD:83:5489:01 I
TMI-l RECOVERY - RNS RETAINER EXAMINATION MAY 20, 1982 m, i.++., e.
.v.,.a. coo,.ad
. abi.co.aly.
SUMMARY
As part of the TMI-l recovery effort, a RNS retainer was exam.ned at the LRC Hot Cell Facility. Although it was unirradiated, the retainer had been installed in-core since the EOC-4 outage in late 1978. Detailed testing of the retainer and its component parts included:
. visual examinations spring load-deflection and full-compression tests sodium azide spot tests liquid penetrant checks l
. bend tests metallography and SEM examinations e
chemical analysis of surface wipe samples 1
While sulfur compounds were found on the external retainer surfaces, there was no evidence of mechanical property degradation or sulfur assisted intergranular attack.
DISTRIBUTION (CCMPANY LIMITED) This information is freely available to all Company personnel. Written approval by the sponsoring unit's R&D coordinator is required only when release outside the Company is requested.
DISTRIBUTION:
R&DD NPGD Bat), DL Inman, SC Baker, RJ (30)
Garner, GL Bhada, RK Library /LRC (2)
Carey, RO Piascik, RS CIS/ ARC Lib 7 (3)
Lynch, ED Culberson, DG Stein, KO Mayer, JT DeMars, RV Uotinen, VO Davis HH Engelder. T Project File Dideon, CG Shield, WA e-/ n ? -
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o BABCOCK & WILCOX RDD:83:5489:01 Page 1 ACKNOWLEDGMENTS r-The authors greatly appreciate the contributions of J. E. Bullard (chemical analysis), V. D. Downs (scanning electron microscopy), and B. J. Parham (metallography) to the successful completion of this effort.
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BABCOCK & WILCOX RDD:83:5489:01 Page 2
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fN 1.
INTRODUCTION
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Analysis of cracked tubes from both A and B steam generators at TMI-l indicated the failure mode was intergranular stress corrosion cracking with a reduced form of sulfur most likely acting as the corrosive agent.1 Since the tube cracks were initiated from the ID surface, the presence of sulfur contaminents f'
in the primary system implies the potential for material degradation of other RCS components.
A detailed examination of a regenerative neutron source (RNS) retainer from the TMI-l core was conducted at B&W's Lynchburg Research Center as part of an effort to assess potential damage to various core components.2 Although the o
retainer was unirradiated, it had been installed during the end-of-cycle four I
outage, and the retainer spring and load legs had been in a stressed condition while exposed to the RCS environment. A RNS retainer was selected for exami-
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f-nation since it contained materials representative of a wide range of core components (304 SS, 308 SS weld metal, and Inconel X750).
After receipt at the LRC, the retainer (#L106) was visually examined and load-deflection tests of the spring were performed. The retain was then dis-I' assembled and the following tests were conducted on the components:
detailed visual examination a
spring compression test a
sodium azide spot tests a
a liquid penetrant checks L
o bend tests metallography o
o SEM examinations Chemical analyses were also performed on cloth wipe samples from the retainer components and on samples obtained at the reactor site. Wipe samples taken at TMI-l were from the north face of a new fuel assembly (NJ0132) and from the retainer, prior to shipment.
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BABCOCK & WILCOX RDD:83:5489:01
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This letter report presents results from the examination of the retainer at the LRC and the chemical analysis of.the cloth wipe samples.
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r-BABCOCK & WILCOX RDD:83:5489:01 Page 4 EXAMINATIONS AND RESULTS,4 2.
3 2.1 Visual Examinations 2.1.1 Method Visual examination of the retainer and its component parts was conducted at magnifications up to 60X with a stereo microscope. Photographic records of visual observations were taken with a 4XS camera attached to the microscope.
Macrophotographs of the retainer were taken with a MP-3 copy camera.
2.1.2 Results A visual inspection of the retainer, prior to disassembly, showed no cracks in the weld, knee, or foot regions of the retainer legs. A schematic view of a I
retainer identifying its various components is shown in Figure 1.
Typical macrophotos of the leg weld, knee, and foot regions are shown in Figure 2.
Virtually no crud was observed on the outside surface. Overall views of the
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retainer are shown in Figures 3 and 4.
After disassembly all retainer components were examined in detail. Disassem-bly consisted of cutting the top fitting off the can and cutting the numbered leg from the hub through the veld area. Examination of the retainer legs showed no cracks or evidence of sulfur assisted attack of the surfaces.
Sev-eral areas of black and white deposits and two small areas of yellow deposits were noted. The black areas are most likely crud and the white areas appear to be boron crystals from the coolant. Attempts to, identify the composition of the yellow deposits by SEM/EDAX analysis were unsuccessful, and the previously 4
reported compositions were obtained from a contaminated sample. Other EDX analyses on similar deposits found on the reactor vessel o-ring indicate the
~
composition is mostly Fe with some Cr.5 The spring surface was a uniform dark gray with localized areas of black and white deposits (see Figure 5). Two small areas also had yellow deposits similar to those found on the retainer leg.
Examination of the retainer can showed no signs of surface degradation.
The outside of the can had a thin, black oxide layer with a blue tint. The in-m.
side of the can had a dark, powdery crud layer with several areas of localized crud deposits.
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BABCOCK & WILCOX RDD:83:5489:01 Page 5 2.2 Spring Load-Deflection Tests 2.2.1 Method Prior to disassembly the X750 spring was tested for preload and spring rate using a load-deflection test rig previously used for irradiated retainers from Oconee 3.6 The retainer spring was compressed using known weights of up to 100 pounds, while spring deflection was mecsured with two dial indicators accurate to 0.001 inch.
2.2.2 Results Three load-deflection curves were recorded and are shown in Figure 6.
Measured spring preloads ranged from 40 to 41 pounds and spring rates from 47-50 pounds
.per inch. These values are considered normal and agree with other retainer s.
data; 7,
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2.3 Spring Compression Test 2.3.1 Method 4
After the retainer was disassembled, the spring was compressed to its solid spring height using five lead bricks. Eack brick weighed a nominal 26 pounds.
Relaxed spring height was measured before and after full compression with dial calipers accurate to 0.001 inch.
2.3.2 Results Relaxed spring height before and after full compression was 4.00 inch, indicat-ing no plastic deformation occurred during testing. After testing, the outer surface of the spring was visually examined at 10X magnification with a stereo microscope. No cracks or other forms of damage were observed.
2.4 Sodium Azide Spot Tests 2.4.1 Method 7
' Sodium azide spot tests for the presence of reduced forms of sulfur were con-ducted by placing drops of test solution on surfaces of interest (spring, leg,
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BABCOCK & WILCOX RDD:83:5489:01 Page 6 i _.
weld area, inner and outer can surfaces). The areas where the drops were placed were then ' observed through the stereo microscope. Bubbles from the solution i r indicate the presence of reduced forms of sulfur (sulfide, thiosulfate, etc.).
The basis for the test is the catalytic acceleration of the iodine-azide re-action by reduced forms of sulfur. This. reaction evolves free nitrogen gas to
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produce bubbles and will detect reduced forms of sulfur at concentrations less than one ppm.
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2.4.2 Results Outside surfaces of the retainer components showed positive reactions to the sodium azide spot test. The inner surface of the can and the retainer spring showed negative reactions. Results of the tests are summarized below:
m Retainer Component P
Run Spring g
Leg-Weld Can (outside)
Can (inside) 1 neg.
- pos, neg.
pos.
neg.
1 neg.
- pos, pos.
pos.
neg.
Tests indicated the presence of reduced sulfur on outer surfaces of the retain-7-
er.
The inside of the can and the Inconel X750 spring showed no evidence of reduced sulfur, but results may have been affected by crud deposits.
~
2.5 Liquid Penetrant Tests 2.5.1 Method Liquid penetrant tests were conducted on the retainer leg and hub and on the spring using the procedure specified in Reference 6.
The pieces were ultra-sonically degreased with tichloroethylene, cleaned with Spotcheck Cleaner /
Remover, and dried with clean cloths. The parts were sprayed with Spotcheck Penetrant and kept thoroughly wetted for 20 minutes. The spring was tested while under compression to open any cracks that may have been present. After removing excess penetrant, the parts were uniformly covered with Spotcheck a
developer and visually inspected.
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BABCOCK & WILCOX RDD:83:5489:01 Page 7 2.5.2 Results No indications of cracks were observed in either the leg, weld area, or spring.
The only positive indications observed were from elongated surface inclusions on the sides of the leg.
2.6 Bend Tests 2.6.1 Method Bend tests were performed on the leg / hub weld region and a 1-1/2 inch piece from the middle coil of the spring. The parts were clamped in a vise and bent to open any cracks which may have been present, r
i 2.6.2 Results The leg weld was bent through approximately 45 degrees with no visible crack 7-initiation, indicating a sound wald. The spring sample was bent and fractured.
The fracture surface was examined with an SEM to characterize the mode of failure. The SEM examination showed the fracture surface was new and failure was 100 percent ductile.
Examples of the appearance of the fracture surface are shown in Figure 7.
No evidence of intergranular cracking was observed.
2.7 Metallography 2.7.1 Method Samples from the leg, knee, weld area, and the active coil and contact region of the spring were mounted in Buehler Epomet. The samples were ground flat on silicon carbide through 600 grit and polished with alumina. Final polishing l
was done with 0.05 aicron alumina. The samples were then metallographically l
examined at 400X magnification for evidence of intergranular attack. The samples were examined in both polished and etched conditions. The Inconel 4
X750 spring material was etched with copper regia and the 304 and 308 stainless steel samples with glycerol regia.
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BABCOCK & WILCOX RDD:83:5489:01 Page 8
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2.7.2 Results The microstructure of all the samples appeared normal and no evidence of inter-granular attack was observed.
Figure 8 shows typical etched micrestructures of the 304 SS base metal, 308 SS weld metal, and X750 spring. The weld area and heat-affected zone are shown at 50X in Figure 9.
2.8 Chemical Analysis of Surface Wipe Samples 2.8.1 Method Cloth wipe samples were taken from the RNS retainer and a new fuel assembly, NJ0132, at TMI-2 prior to shipment of the retainer to the LRC. The retainer wipe covered 15.5 square-inches of the leg area. The fuel assembly wipes covered one face of : grid and across 15 rods just below a grid. Wipe samples were taken from the retainer after disassembly at the LRC.
Samples were ob-tained from one retainer leg, two coils of the spring, and the inner and outer surfaces of the can.
Wipe samples from the disassembled retainer were analyzed for chlorine content by a LRC procedure similar to ASTM D512. " Tests for Chloride Ion in Water and Waste Water," and for sulfur content by a procedure similar to ASTM D516. " Tests for Sulfate Ion in Water and Waste Water." Since the chloride ion results were low (8 pg total or less) and_used half the wipe sample, wipe samples from TMI-1 were only tested for sulfate content.
2.8.2 Results Chloride and sulfate ion contents of wipe samples from the retainer parts were
- low,
< 5 to 8 pg total Cl and < 20 to 50 pg total S0
. When the back-2 ground from the cloth samples was subtracted, only the sample from the spring showed any removable sulfur. Results of the sulfate analysis of wipe samples are given below:
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BABCOCK & WILCOX RDD:83:5489:01 Page 9
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LRC Wipe Sample Results (cloth batch 67)
RNS Total Less Total
<20 20 Leg
<20 Spring 50
>30
>20 9
42 I
Can 25
>5
>3 28 (outside)
Can
<20 (inside)
- on a whole cloth basis Cloth wipe samples taken from the retainer after it was removed from the core and from the fuel assembly grid and rods showed slightly higher levels of re-2
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movable sulfur, in the range of three to five pg/in. Results of the sulfate analysis are given below:
TMI-l Wipe Sample Results Cloth Total Less Total Wipe Removable
~
Batch Sample SO4, pg Blank Sulfur, Ug Area, in2 Sulfur, ug/in2 75 blank 30 blank
< 10 Avg
<20 Zr Fuel 50
>30
> 10 2.7 N4 Rods r-Inconel 90
>70
>23 8.1
%3 Grid 71 blank
<10 blank 20 Avg
<l5 Cloth 20
>5
>1.7 Dipped in core Retainer 243 228 76 15.5
%5
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=
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CONCLUSIONS While reduced forms of sulfur were detected on the retainer components, there was no evidence of mechanical property degradation or intergranular attack.
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BABCOCK & WILCOX RDD:83:5489:01 Page 11 4.
REFERENCES r
1.
M. A. Rigdon and E. B. S. Pardue, " Evaluation of Tube Samples from TMI Final Report," RDD:83:5390-03:01, Babcock & Wilcox, Lynchburg, Virginia, 7-April 1982.
2.
C. G. Dideon to D. G. Culberson, Memorandum, "TMI-l Recovery - Core Exami-nation Task," FPO-82-41, March 24, 1982.
1 3.
W. A. McInteer and G. M. Bain to Distribution, Memorandum TMI Core Re-covery - Initial Retainer Exam," April 30, 1982.
r--
f, 4.
W. A. McInteer to C. G. Dideon, Memorandum, "TMI Core Recovery - RNS Re-tainer Detailed Exam," May 6, 1982.
5.
D. L. Baty, " Examination of TMI-2 Reactor Vessel 0-Ring and CRDM Closure Insert," RDD:83:5490/5491:01, Babcock & Wilcox, Lynchburg, Virginia, May 25, 1982.
6.
E. B. S. Pardue, " Examination of Oconee 3 RNS Retainers," LRC 9085, Babcock
& Wilcox, Lynchburg, Virginia, February 1982.
7.
F. Feigl, Laboratorv Manual of Spot Tests, p. 163-166 Academic Press, New York, 1943.
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13 FINAL REPORT on o
Sp FAILURE ANALYSIS OF INCONEL 600@
t TUBES FROM OTSG A AND B OF THREE MILE IST.AND UNIT-1 to GPU-NUCLEAR June 30, 1982 by Arun K. Agrawal William N. Stiegelmeyer Warren E. Berry e
2 BATTELLE Columbus Laboratories 505 King Avenue Columbus, Ohio 43201 mn
~ h n ;r 2'
A C/
tvw -
l TABLE OF CONTENTS Zagi
1.0 INTRODUCTION
1 2.0 APPROACH........
2 3.0 RESULTS OF NON-DESTRUCTIVE EXAMINATION.
3-1 3.1 Introduction 3-1 3.2 Radiation Level Check......
3-1 s I 3.3 Visual and Photographic........
3-1 3.3.1 Results 3-1 3.3.2 Significant Observations............
3-14 3.4 X-ray Radiographic Examination 3-14 3.4.1 Results 3-14 3
3.4.2 Significant observations.
3-19 3.5 Eddy Current Examination 3-21 3.5.1 Results 3-21 3.5.2 Significant Observations.
3-21 4.0 RESULTS OF OTHER EZAMINATIONS 4-1 4.1 Tube B-8-25.....................'.
4-1 4.2 Tube B-11-23 4-18 r
l 4.3 Tubes A-23-93, A-88-11 and A-112-5 4-25 i
4.4 Tube A-71-126.....................
4-31 4.5 Tube A-146-6 4-43 4.6 Tube A-146-8 4-64 5.0 RESULTS OF y-RAY ISOTOPIC ANALYSIS.
5-1 6.0 DISCUSSION.
6-1
7.0 CONCLUSION
S 7-1 8.0 ACKNOWLEDCMENTS 8-1 J
LIST OF FIGURES Paee Figure 1.
Appearance of As-Received Tube B-8-25 at 0, 90, 180 and 270 Degree Positions.
3-3 Figure 2.
A Closeup View of the Dryout Marka on Tube B-8-25 at 90 Degree Position.
3-4 Figure 3.
Appearance of As-Received Tube B-11-23 at 0, a.
90, 180 and 270 Degree Positions.
.3-5 Figure 4.
Appearance of As-Received Tube A-23-93 at 0, 90, 180 and 270 Degree Positions.
3-6 Figure 5.
A Closeup View of the Dryout Marks on Tube A-23-93 at 90 Degree Position 3-7 Figure 6.
Appearance of As-Received Tube A-71-126 Segment 1 at 0, 90, 180 and 270 Degree Positions.
3-8 Figure 7.
Appearance of As-Received Tube A-71-126 Segment 2 at 0, 90, 180 and 270 Degree Positions.
3-9 Figure 8.
Appearance of As-Received Tube A-71-126 Segment 3 at 0, 90, 180 and 270 Degree Positions.
. 3-10 Figure.9.
Appearance of As-Received Tube A-71-126 Segment 4 at 0, 90, 180 and 270 Degree Positions.
. 3-11 F18ure 10.
Appearance of As-Received Tube A-71-126 Segment 5 at 0, 90, 180 and 270 Degree Positions.
. 3-12 Figure 11.
Appearance of As-Received Tube A-88-11 at 0, 90, 180 and 270 Degree Positions.
. 3-13 Figure 12.
A Closeup View of the Dryout Marks on Tube A-88-ll at 0 Degree Position.
. 3-15 Figure 13.
Appearance of As-Received Tube A-112-5 at 0, 90, 180 and 270 Degree Positions.
. 3-16 Figure 14.
Appearance of As-Received Tube A-146-G at 0, 90, 180 and 270 Degree Positions.
. 3-17
~
Figure 15.
Appearance of As-Received Tube A-146c8 at 0, 90, 180 and 270 Degree Positions.
. 3-18 Figure 16.
Photograph of As-Cut Slices Al through A8 From Tube B-8-25 4-3 Figure 17.
Photomicrographs of the Cross-Section of Bent Specimen A2 from Tube B-8-25.............
4-4
~
l LIST OF FIGURES (Continued)
Pace Figure 18.
SEM Photographs of the Fractured Surface of Specimen A6 from Tube B-8-26.
4-6 Figure 19.
TEM Photomicrographs of the Replica of Fracture Surface of Specimen A4 from Tube B-8-25 After Descaling 4-8 Figure 20.
SEM Photograph of the Apex of U-Bend of Specimen A7 from Tube B-8-25 4-9 Figure 21.
Photograph of Specimen B from Tube B-8-25 Showing Multiple Fracture Surfaces Stacked Together For ESCA Analysis
. 4-14 Figure 22.
A Tree-Like Brown Deposit on the ID Surface of Tube B-8-25
. 4-17 Figure 23.
Photomicrograph of IGC in Specimen E from Tube B-ll-23 4-20 Figure 24.
Photomicrograph of IGA in Specimen E from Tube B-11-23
. 4-21 Figure 25.
Photomicrograph of Specimen A from Tube B-11-23 Showing IGC and Severe IGA on Either Side of the Crack
. 4-22 Figure 26.
Photomicrograph of IGA on the ID Surface of Specimen A frem Tube B-11-23.....
. 4-23 Figure 27.
Photomicrograph of the Microstructure of Specimen A from Tube B-11-23.........
. 4-24 Figure 28.
Photograph of the Descaled Specimen F from Tube A-71-126 Showing Heavy Scoring
. 4-35 Figure 29.
Photograph of ID Surfaces of Two Halves of Tube A-71-126 Between 51.0 and 60.0 Inch Before Descaling; A) 45' B) 135' C) 225' D) 315* Face.
. 4-36 Figure 30.
Photomicrograph of the Transverse Cross Section of Specimen I from Tube A-71-126...
. 4-37 Figure 31.
Photomicrograph of the Longitudinal Cross Section of Specimen J from Tube A-71-126..
4-38 Figure 32.
Photographs of ID Surfaces of Two Halves of Tube A-146-6; A) 315* B) 225' C) 135' D) 45' Face.
4-45 Figure 33.
Photomicrographs of the Microstructure of Three Different Regions of Specimen B from Tube A-146-6
. 4-47
+
LIST OF FIGURES (Continued)
Page Figure 34.
Microhardness Values at 8 Different Sub-Locations on Sp *cimen B from Tube A-146-6...... 4-48 Figure 35.
Photomicrograp' of Through Wall IGC in Specimen C frc.' Tube A-146-6 4-49 Figure 36.
SEM Photomicrograph of a Brown Spot and White Deposit on the ID Surface of Specimen D from Tube A-146-6 4-50 e
i Figure 37.
SEM Photograph of an IGA Pit on Descaled Specimen D from Tube A-146-6 4-51 Figure 38.
Photomicrograph of the Cross Section of a Pit in Specimen D from Tube A-146-6...........
4-53 Figure 39.
Back Scatter Electron Image and X-Ray Images of Elements T1, S, Cr, Ni and Fe of a Pit in Specimen G from Tube A-146-6 4-54 Figure 40.
Relative Ion Intensity Versus Sputtered Depth in SIMS.......................
4-63 Figure 41.
Photcgraphs of ID Surfaces of Two Halves of Tube A-146-8; A) 45' 3) 135' C) 225' D) 315' 4-66 f
Figure 42.
Photomicrographs of the Microstructure of Two
[_
Different Regions of Specimen B from Tube A-146-8..
4-67 4
Figure 43. Microhardness Values at 8 Different Sub-Locations on Specimen B from Tube A-146-8...........
4-68 Figure 44.
SEM Photograph of a Brown Decoration on the ID Surface of Specimen E2 from Tube A-146-8 4-70 Figure 45.
SEM Photograph of a Crusty Deposit in a Brown Spot on the ID Surface of Specimen El from Tube A-146-8 4-71 Figure 46.
SEM Photograph of the Fracture Surface of Specimen E2 frem Tube A-146-8 4-72
~
Figure 47.
Photomicrograph cf an ICC in Specimen El from Tube A-146-8 4-73 Figure 48.
SEM Photograph of a Shallow Pit on the ID Surface of Specimen I from Tube A-146-8...........
4-75 Figure 49.
SEM Photograph of a Descaled Pit on the ID Surface of Specimen I from the Tube A-146-8....
4-76
i LIST OF FIGURES (Continued)
Page Figure 50. Photomicrograph of an IGA on Specimen G from Tube A-146-8..................
4-77 Figure 51. Photomicrograph of an IGC in Longitudinal Cross Section of Specimen A from Tube A-146-8....
4-78 Figure 52.
Photomicrograph of an IGC in Transverse Cross Section of Specimen C from Tube A-146-8.......
4-79 LIST OF TABLES Page r-Table 1.
Defect Indications in Radiographs of Tubes from THI-1 Steam Generators A and B.
3-20 Table 2.
Results of EC Examination of Tubes from TMI-1 Steam Generators A ar.d B Using Differential and Pencil Probes....
3-22 Table 3.
Examination Results of Tube B8-25 4-2 t
Table 4.
EDAX Analysis of Fracture Surface of Spacimen A6 from Tube B-8-25 4-7 Table 5.
AES Analysis of Fracture Surface of Specimen A3 from Tube B-8-25 4-11 Table 6.
ESCA Anclysis of Fracture Surface of Specimen A3 from Tube B-8-25 4-12 Table 7.
- ESCA Analysis of Fracture Surf ace of Specimec B from Tube B-8-25..................
4-15 Table 8.
ESCA Binding Energies and States of Elements on Specimen B from Tube B-8-25 4-16 Table 9.
Examination Results of Tube B-11-23 4-19
'~
Table 10. Wall Thickness of Tube B-11-23............
4-26 Table 11.
Examination Results of Tube A-23-93 4-27 Table 12.
Examination Results of Tube A-88-ll 4-28 Table 13.
Examination Results of Tube A-ll2-5 4-29 Table 14.
Wall Thickness of Tube A-23-93............
4-30 Y4
i ed LIST OF TABLES (Continued) e-Page Table 15.
Examination Results of Tube A-71-126
. 4-32 Table 16.
Composition cf Tube A-71-126 Alloy
. 4-40 Table 17.
ESCA Analysis of ID Surface of Specimen C frem Tube A-71-126
. 4-41
[
Table 18.
ESCA Binding Energies and States of Elements on Specimen C from Tube A-71-126
. 4-42 i
Table 19. Examination Results of Tube A-146-6......
. 4-44 i
Table 20.
ESCA Analysis of ID Surface of Specimen F2 from Tube A-146-6..................
4-55 m.
! ^
Table 21.
ESCA Analysis of ID Surface of Specimen Fil from Tube A-146-6.
. 4-56 Table 22.
ESCA Analysis of ID Surface of Specimen E from Tube A-146-6
. 4-57 Table 23.
ESCA Binding Energies and States of Elements on Specimen F2 from Tube A-146-6............
4-59 Table 24.
ESCA Binding Energies and States of Elements on Specimen Fil from Tube A-146-6
. 4-60 Table 25.
ESCA Binding Energies and States of Elements on Specimen E from Tube A-146-6
. 4-61 Table 26.
Examination Results of Tube A-146-8.........
4-65 Table 27.
Gamma Ray Isotopic Analysis Results..
5-2 c
W w
ts
FINAL REPORT on FAILdREANALYSISOFINCONEL600#
TUBES FROM OTSG A AND B 0F f'
THREE MILE ISLAND UNIT-1 to GPU-NUCLEAR from l
t BATTELLE Columbus Laboratories June 30, 1982 by 1
l Arun K. Agrawal, William N. Stiegelmeyer Warren E. Berry INTRODUCTION Three Mile Island-Unit 1 power plant was brought to hot functional status between August and September of 1981 af ter a long cold shutdown for about two and a half years. The plant was brought back to cold shutdown status and was then hydrotested in November of 1981. On November 21, 1981 small leaks from primary side to secondarf side were detected in tubes of the once-through-steam-generator (OTSG).
Subsequently, leaking tubes were identified by bubble test and eddy current examination.
Eddy current examination indicated defects also in some other tubes. As a result, a few tubes with defect indications were removed, along with known leakers, from OTSG-B for determining the nature of the' defect (s).
Two tubes from OTSG-B, identified as B-8-25 and B-11-23 were i
j received at BCL on December 28, 1981 for failure analysis. Tube B-11-23 1
~
~.--
2 was a known leaker; a quick metallographic examination of the defect in this tube estah11shed that the failure was due to intergranular stress-l
~
corrosion crackins (IGSCC), and the IGSCC had initiated on the inside surface of the tube.
While detailed examinations of the two tubes were proceeding, t.
two more shipments of tubes pulled from the OTSG-A were received at BCL for similar examinations. The first snipment from GPU-Nuclear was
[
received at BCL on January 21, 1981; it contained four tubes with identifications A-71-126, A-88-ll, A-112-5 and A-146-8.
The second
(
{
shipment contained two tubes with identifications A-23-93 and A-146-6; this shipment was received on January 27, 1982.
[~
All the tubes shipped to BCL were from the upper tubesheet
~
(UTS) region of OTSGs A and B.
Tubes B-8-25, B-11-23, A-23-93, A-88-11,
['
A-ll2-5, A-146-6 and A-146-8 were "short-pulls", i.e., these were approximately 12 to 12.5 inch long segments cut from the upper tubesheet crevice region.
Only one tube, A-71-126, was a "long-pull", i.e., it included sections of the tube from beyond the UTS crevice. This tube was received in five segments, labled A-71-126(1) for the top section and then sequentially up to A-71-126(5) for the bottom-most section. The total combined length of all the five aegments was 68 inches.
This report contains the results of various examinations conducted on the above tubes at Battelle. Probable cause of the attack also has been identified APPROACH The detailed failure analysis program for TMI-Unit-1 tubes was developed in close censultation with GPU-Nuclear personnel. There were two main objectives in this program: 1) to identify and characterize the nature of defect (s) in various tubes, and 2). to determine the probable cause(s) of attack which produced the defect (s). A third objective of the program was to identify, based upon the plant history data provided by GPU-N, the environmental condition (s) which may have been responsible for the attack.
-c
~
V 3
The broad base failure analysis program consisted of the following examinations and tests:
i Nondestructive erarination (NDE)
Meta 11ography and Microstructural examinations f.
Microanalytical surface examination and Physical tests.
The NDE included visual and photographic inspection, X-ray
~
7 radiography and eddy currect (EC) inspection.
The EC inspection used two L-different types of probes: a standard probe (i.e., differential probe)
[-
and an absolute probe (i.e., pencil probe).
The pencil probe was used to specifically inspect the roll transition region, i.e.,
the area
[
between the rolled section and the unrolled section of a tube.
1 Radiography was used to locate defects that produced sufficient discontinuity in the tube wall for a relatively easy penetration of X-rays. For example, the technious was very helpful in locating the j '
through-wall, but not easily visible, crack in tube 3-11-23.
I I'
There were a few tubes which had obvious " lip-cracks", i.e.,
I a broken off wall within 0.25 inch of the top end.
These " lip-cracks" were photographed for documentation purposes, t
Meta 11ographic and microstructural examination involved examining longitudinal and transverse cross section of specimens h.
removed from different locations of various tubes. Specimens were examined in the as-polished condition and some af ter etching with nital
~i or phosphoric acid. Some specimens were examined in the scanning electron microscope (SEM). One fracture surface was examined with the transmis-sion electronmicroscope (TEM).
In order to determine the nature of corrodent' responsible for the attack, surfaer, compositions of several tuhe specimens were investigated.
t Both the inside diameter (ID) surface and the attacked area, e.g.,
fracture surface were analyzed. Techniques used in microanalysis of surfaces were energy dispersive X-ray analysis (EDAX), Auger electron spectroscopy (AIS),
electron spectroscopy for chemical analysis (ESCA), secondary ion mass w-
'M
i 4
spectroscopy (SIMS) and electron microprobe analysis (EPMA) for X-ray
~
images of elements. I-ray differaction (IRD) also was used for corrosion
~
product identification.
Bulk composition of tube material also was determined. X-ray c
fluorescence and other standard methods were used for this purpose.
h Physical tests of tubes or tube material included, 1) tension test; 2) wall thickness measurement and 3) microhardness measurement using Knoop diamond pyramid tester.
The susceptibility of a few tubes to intergranular attack (IGA) f by polythionic acid was investigated using the electrochemical potentio-kinetic reactivation technique (EPR).
{ '-'
In support of the failure analysis program, five wipe samples from OTSGs A and B were also supplied by GPU-Nuclear. These were analyzed using y-ray isotopic analysis for the determination of active isotopes I
present in OTSGs.
4 f
1
~~
b W
~
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- h
- iT T T* '- - -
" ' ' * ' ' * ~ - - - - - - - - - -
i 3.0 RESULTS OF NONDESTRUCTIVE EXAMINATION 3.1 Introduction d
Tube segments from GPU-Nuclear were received packaged in 40 gallon drums. Af ter opening the packages, each tube segment was subjected
~.r-to four different nondestructive examinations (NDEs).
The NDEs performed F
were:
- r --
(1)
Radiation level check
'L.
(2) Visual and photographic j.-
j; (3) X-ray radiographic (4)
Eddy current inspection i
3.2 Radiation Level Check i-The radiation level of each tube segment was checked to establish
,5 safe working conditions. The radiation level at contact for different tubes ranged between 20 mR/hr and 40 mR/hr. The above radiation levels were considered low, nonetheless, appropriate safety precautions were
'[
still required when working with these tubes, in order to pcotect both personnel and work facilities from radioactive contamination.
I 3.3 Visual and Photographic
. I, 3.3.1 Results.
Initial visual inspection of tubes (segments) showed no obvious defects in the form of a crack or a pit on the OD surface, except for the dryout water marks and some scratch marks; the latter prob-L.
ably were from the tube cutting and pulling operations. Tube ends in a
~
few cases, however, were more ragged than in others, this again was con-
~
sidered to be a result of tube removal operations.
Tube defects in the form of lip-cracks were observed at the upper (top) end of tubes A-88-ll, A-112-5 and A-146-8.
The lip-crack in each case was associated with the 0* orientation slot cut in the tube.
a.s g....
.g.
~
2 Following the initial visual inspection, each tube was photo-r_
graphed in four different positions, i.e., 0*, 90*, 180* and 270*.
An inch scale also was photograghed along side of each tube to show its length.
.)
Photographs of tube B-8-25 are shown in Figure 1; water marks are visible along the whole length of the tube and in all four positions, 2
1.e., 0*, 9 0*, 180* and 270*. A closeup view of the dryout mark at 90*
I
!2 is shown in Figure 2.
~
gr-Photographs of tube B-11-23 are shown in Figure 3; water marks
{ i.,
are visible along the whole length of the tube and in all four positions.
f,,
The 270* quadrant, however, was relatively cleaner than the other three a
quadrants.
Photographs of tube A-23-93 are shown in Figure 4 with water j
marks visible along the whole length of the tube and in all four positions.
A closeup view of the top end at 90* position is shown in Figure 5.
Some vertical scratch marks are clearly visible in the rolled section (0-1.0 in.)
of the tube. The end of the rolled. section is indicated by the circum-ferential white ring at 1.0 inch.
Tube A-71-126 was a long-pull and it was received at BCL in five segments. These seg=ents were marked 1 to 5, in the order in which they were removed from the OTSC, i.e.,
1 for the top segment and 5 for the bottom most.
Photographs of segmencs one through five are shown in i
Figures 6 through 10, respectively. Water marks on tube A-71-126 were less extensive and dense, particularly those on lower segments, than those observed on the previous three tubes. However, all four quadrants of the five segments of tube A-71-126 showed some water spots. No particular quadrant was free of water spots.
Figure 7 for_ tube A-71-126 seg=ent 2 shows circumferential shiny ring pattern over most of the tube surface, particularly in the first 7 inches of the segment. These rings are obviously from the mechanical operation of tube removal, but such an extensive =arking was not observed on any other tubes.
Photographs of tube A-88-ll are shown in Figure 11, water marks on the O' quadrant are relatively heavier than en the other three quadrants.
- ^ ^
)
I i
i J
i 90*
u 180' k' 5; ei;.
ij (.it' l r l j '.. ' ;t L l 8 sp :t t
- i >
f-f i.i
'I 4r 7
'9 to 11 l
2
- 5,, '
1 i!
i 270*
1 FIGURE 1.
APPEARANCE OF AS-RECEIVED TUBE B-8-25 AT 0, 90, 180 AND 270 DEGREE POSITIONS
4 s
~
r i
e-1 O
\\
FIGURE 2.
A CLOSEUP VIE'J OF THE DRYOUT MARKS ON TUBE 3-8-25 AT 90 DEGREE POSITION i
4 a ~g i
.t i
t i
s
,y_
r;
,4 i.g_-
,e
..c :
7.s
.{.
' T '; 4.
7 90*
4 4
9 e
g
.~%.
- g. _,,_.
,..A.,,,,
- g.. ~ s
- i.. 0;
. f..
-~,.=,,n,...-~..
i FIGURE 3.
APPEARANCE OF AS-RECEIVED TUBE B-11-23 AT 0, 90, 180 AND 270 DECREE POSITIONS l
. )
i 1
.q l
l i4 M N'd iP 7M -
13 s
l'il.M '81 ') t) fri
~
lI
' j;,1st'
+
v' 180* "'~'
j i:.,tj H F'iy] i l'iily i p'lil pu cj l]hi[8. p;;p{pj.!:$p'...,
l l
ilji
,.; o,,
.5. !
(d ' -
'7 9
t lo t
3 cl:
lit
....-.-..- _..,.1 1.
- ~
i M mi fr
,i 270*
.IJ 0 V!!K l. "i iWl ih i,j ; 7; cj.l{pjhfl jiff-Qij.l@hjdO;i,.i! :!! 'k
- pj ;;'.;...,12!
e,,,i 13.
i i
1 2
.1,,
1-8
'9 i 10 I 6'
i 51 11' FICURE 4.
APPEARANCE OF AS-RECEIVED TUBE A-23-93 AT 0, 90,180 AND 270 DEGREE POSITIONS i
m 1
7 l.
' I.
i 6
8
-e.,
a 4
.p t.
- - m' V~
em 0
A 06e
- - ~
l m'
+"
h Ii
- j -
.g
+
+
he 4
2 I
i FIGURE 5.
A CLOSEUP VIEW OF THE DRYOUT MARKS ON TUBE A-23-93 AT 90 DEGREE POSITION
=O m
aw-m-
+-
f 1
i l
t i
i
!4 !! I i.1 i
l ammat /.
==
0*
- ,n.: g,,ig: p :I ;.; og. i.i4;i..pp.,i[igs..
o1 5; i 6 '
'7
! 8 91 ' '
}
1 1
10 11 il 4
- ,. f 1.. 1
?
I M *fi 90, g4J
,1 e.
.... % w g, i
- 4
, j T ;- '
j' 8 ; i ilg:'p <,'
(
'7i. ';.p p.p.
i i.
t I
~5--. '...fi t
91 10 11:
1.:
i i
l l
l
[
Pil /f 1 t.
t in" i
i 1
180*
l j
- m. j',I,qil. a i [pi:
4, ' 6:. 4.j.c t I
- ,iF c..t i d t
i'i,'i'i:ijUhWf,hfll.i.....
lg o:
j 1
- 2. ;-
'34,
i 1
.t i
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8'.
3 '9:
I. 10 1 1 '_.
t.'
.J
'4
(
I i
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=
m 270*
1 i
'-l i j.j"{ ni oj i it7i ' j,1 pjl:,,pH,lij t 3,,
1 l
1
- 1.. - !
8 9
'10...
_ 11.:_I.. t.i..
1.1..
7 3-
. -. -.. 6.
{
1
]
FIGURE 6.
APPEARANCE OF AS-RECEIVED TUBE A-71-126 SEGHENT 1 0, 90, 180 AND 270 l'
t
]
DEGREE POSITIONS j
ii j
!i l
4 f
l
gm 3
7 g
t g
i i
i i
ni.m u.
'I 1"I ?l LY.-? - 97'
!. I I
2 j.3 I
j l
ni n.i:r,
- s w j
e i
l l
i l y / l - lif, '
_m-
- i.
! l j
l 3_
1 FIGURE 7.
APPEARANCE OF AS-RECEIVED TUBE A-71-126 SECHENT 2 AT 0, 90,180 AND 270 DEGREE POSITIONS f
1 t
I
1 a
.- q 2
0*
.--s..,.,...
...-.-.ma....'a.-.....,a..
- L
.-.a......,
o,. 4'I i
3 I
6 7
. Il 9;
lo
_10 '
.tr _
13 90*
1 w'. 4 1
,,U, a
.f ij i
i 1
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[+
a-6 7
11 9:
la s>
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'I i-i 180*
i I
i a+
tv 7,
11 1 ' 9.
10
_.1 1. !..',_1.._!
t.)
^
270*
i""--
e
........... _ u. m _i L c a' 2
m..
. w.
u.'
-r -'
...--.".'m" ' ' ' - " ' - - - - - _... '. '.
If
.. _. '_... _ _ _ _6... _,__' 7 ;
' 11
, fI I
'1
, +{f.
e-j,
l 5
9:
10
_. _ _1 1_ :_.'... _.t i 1.i FIGURE 8.
APPEARANCE OF AS-RECEIVED TUBE A-71-126 SECHENT 3 AT 0, 90,180 AND 270 DEGREE POSITIONS l
I j
j i
m. -..
...;,,,n...
p,,. ~.... g
,5'l,o,b t.
-- (
4 i
=t-r t,.i
[
h'
~
.j 0*
H gl l
i 9] 551 M
,.]!( i 'l l!j g 7j;hil'.i.8. f l!. '9 ' ' '10
? ! ;-lit >' <.12f
'13:
li!
si 4 d ta.,
- ,i;.,iUpn,jd$.-
!;i
>!.o
.,3'- y-3
- 6. > -
1 t
~-
il.
s 5'
hl
!N /}-13, '4 - HP iH
- ~... - _. _
. _. - _. ~... _,,. _ - -,
t v
't 17.1 ll-1:t 4-lW H
...-,____.L,._,4.,
I I
.t 6
f ut fl g. i,4 t '. i -
i, H t
270*
.?
L l-.
i.:" ] 5:rl j'p[ Sdp.py) p,q ;, 'a iijlfiqlj,pppp. g 3,,
j ;,.
ii
/ 6' l 7t at - I : 9j ' '. 'In t ' !' ]!:
12!
13' I
i I.
FIGURE 9.
APPEARANCE OF AS-RECEIVED TUBE A-71-126 SECHENT 4 AT 0, 90,180 AND 270 DEGREE POSITIONS l
l i
l
a
- -a,.a.a es s.
._a
-_-.e-a
,ahm.a m.
I
. 1 i
l i
t u
init'tM J #
+'
t
(
I or
", ee ttcht i
2 n
. as,se I
l b-
}, t u, s
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p
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v 90*
f- :
)
,(,
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{n
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h.
w, l
c e
r.
PJ
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t t l f. ' li f*
F il
~
1ee r' p
i v 10 a
y : '.'. ' s. p. 5' N ' '
' 6 l 76 '
- 8.,',
7,..
. n.8 !.,11 '
lb!..'Ul3
.l.a. _
j p-3 h',-
' agecott.@ enre 4
!, (
y k'
. 4
~
8 p
m
.e s c <
t.,
270 E m uuu,musuuns en suungu ngu e memu n u ous n
i 7, f j. m..oi.w l r..... m m }it li o r.m1
- [. tg'1 j
-i r.
..o, 4
ts.
t
- o,,. y. -.g :-
...5.._
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t to r { - i 12. -
13' 14 l
\\.
f.i e
21*-- e e.,a ee.
.. es etc as
- ~. :~-
l !
4 l I j
FIGURE 10.
APPEARANCE OF AS-RECEIVED TUBE A-71-126 SEGMENT 5 AT 0, 90, 180 AND 270 ff DEGREE POSITIONS l
1 4
e a.
0 A
t q
-]
}
g j
i 1
1 i
l l
4 l
t
,. -,.) f 33;!gyt,,7 p ~, sm m -,,. -,,
1 r.
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r
'n'
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..., _... _. _ ~.
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g Hi' 1M1 83-11 IM t
180*
)
---.-~ -.
. - ~...
I
'r 1
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, i c
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l'11 c.. ] I Nf lM I
270*
L t
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< _u, 10 i - 14 < a WI... ' U, 1
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1 i
l i
FICURE I1.
APPEARANCE OF AS-RECEIVED TUBE A-88-11 AT 0, 90, 180 AND 270 DECREE POSITIONS I
i 4
i a
=
1
i.
I
)
g s
o,
h.
r A closeup view of the dryout deposits in 0* quadrant is shown in Figure 12.
w c.
The lip-crar.k, described earlier, can bt,seen at the slotted end in the O' photograph.
Photographs of tubes A-112-3, A-146-6 and A-146-8 are shcwn in Figures 13,,14 and 15 respectively.
Dryout water marks are presenti along j
3
'che whole length and in all,four quadrants of these tubes.
Some vertical M
scratch marks in the rolled section of tubes and circumferential water ring at the end of rolled section are also visible in these photographs.
\\s Some scratch marks at 6ther places along the tube length also can be seen
['
i.a Figures 13 and 14'.
L-In Figure 13 a lip-crack can b'e scen extending from the slot in p
tubi A-112-5.
A similar lip-crack is visible in tube. A-146-8 in Figure 15.
a g
S'gnificant Observations. Visual and photographic 3.3.2 i
s f,
a h::
examinatior.s of the CD surface of tubes are su=marized belew:
(1)
D;yoit water mirks were present practically on
}
-all tubes. These marks were present practically
~
on' all four quadrants of each tube.
1 r.
L' (2) Vertical scratches were observed on all tubes at s
s various locations, but the scratches were particularly s
s, s
s. ; hea'vy in the rolled section of each tube.
, {'3) 'Some shiny circumferential ring patterns were observed s
r' V
'.a;
'.on some tubes; the ring patterns were numerous on x., segment 2 of tube A-71-126 and are probably the result of efie tube pulling operation.,
(4)
(ip-cracks were observed in tubes A-88-ll, A-112-5 and l
l A-146-8; the cracks we're associated with 0* orientation
^
l d
slot in each case.
I l
A
_3. _4 X-ra1_ Radiographic Examination
\\,
g 3.4.1 Results. lEach tube sagtent was radiographed individ-ually in four different positions, at approximately 0*, 90*, 180* and
~.
- -- % g w
l
~
l
--- q p
,- - )
)
3 g
i i
i f
. Iv,1 1IJ 5 - m
- : e it -
e 0'
i -
l l
l
?
90*
I3l Illi
- 940 h'7 L
e,
m 180*
~I 1
- -w--*.-
_me,,_.
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,,...g b
d 4
.jh an A Em
%mmM y
270*
'.1 6
I N'ij, 3ll[j! 011ll' pj l j di : !(4!{[8! ;illkij!dillj'Q!
- p{.. ! j ' j gi ' gy p
':ll.u.
l',;A
.a l'
'3'.
]
7l
~
46:
6 FIGURE 13.
APPEARANCE OF AS-RECEIVED TUBE A-112-5 AT 0, 90,180 AND 270 DECREE POSITIONS j
i l
I
I c
.J J
i
's i
l e
s l
h(
- [
J I'll U// l',
d' '
' ='
+!
}
I t
-)
w.,
n
-... -.. a..
.?.*.
-(
l ly:[
q G
/
4 s..
n xh:T i
- ,,7.
1 w
..; c'
. MI,-
r 4
'4
's l'T ).ti-f - W..
fr W
.. _. ~..... _ -
..._rf.._,..
' \\q ? ', %:
-t' r
s
.s
-s
.,.r 4
+
- i' h' 21! ISC l#
hit l
l 180*
]
]'
e,j' ;-
=
- e
1m & t.- h w wi '.,
..a >
?;
270*
i t
FIGURE 14.
APPEARANCE OF AS-RECEIVED TUBE A-146-G AT 0, 90,180 AND 270 DECREE POSITIONS 3
~
'i
-'i J
1 10.'
. TMI 16 s,if '
~
'l i
O' I
j
'u i
s
..:t-1 a
i,c
}xl [y.3..)p
-4,'
1 90*
- - - - - ~ - - - -
.e 3
h ii' IMI14-3 1Af E6I 180 f,
I' I "S ' I E'!
270*
3 FIGURE 15.
APPEARANCE OF AS-RECEIVED TURE A-146-8 AT 0, 90, 180 AND 270 DEGREE POSITIONS I
l 1
[
19 270*.
Then each radiograph was examined over a light viewer to observe
,]
changes in light density over the radiograph's surface.
In several radio-graphs, dark hairlines were observed agains t the light general background.
[3 These dark hairlines were considered as indicative of defects (possibly narrow hairline cracks) in the corresponding area on the tube.
I The hairlines in practically all cases ran in transverse direction o
and covered anywhere from 1/10th to 3/4th of the tube diameter. A defect II shown by a hairline was classified as a " clear" in'dication if the hairline d
was suf ficiently dark, otherwise as a " faint"~ indication. The location
]
of each indication was recorded. All the indications observed on various tubes are listed in Table 1.
No vertical (longitudinal) hairline indications were observed Lj corresponding to the OD surface scratches described earlier in Sub-section 3.2.
This inplies that the scratches were superficial, only surface deposit deep, and did no't scar the metal underneath, otherwise indications would have been obtained.
n u
3.4.2 Significant Observations.
Results of radiographic fl examination of various tubes are summarized below:
l)
(1)
Defect indications for lip-cracks were obtained in (j
tubes A-23-93, A-88-ll, A-ll2-5 and A-146-8.
The indications were faint in tube A-88-ll, but clear in
. tn l{
the other three.
(2) Defect indications in the vicinity of roll transition
-[]
area (i.e., location 0.75 to 1.25 inch) were obtained
'J in tubes A-88-ll, A-112-5, A-146-6, A-146-8 and 7
B-ll-23.
The indication was faint in tube A-146-8 f3 LJ but clear in the other four tubes.
(3) There were setteral clear defect indications in all
,,!j tube segments examined; including segment 5 of tube A-71-126 which was remcved fron below the upper tube sheet of OTSG-A.
U.
I I
g~ -
TJ I'.]
i i
LADLE.1.
DEFECT INDICATIONS IN RADIOCRAPHS OF TUBES FROM THI-1 STEU1 CENERATORS A AND 8
~ ' ~ ' ~ -
Tube Number Defect Location From the Top of the Tube. Inch A-23-93 Lip Crack 2.75-3.25 12.0 12.25 Faint Faint clear A-71-126/1 1.75 12.23 Clear Clear A-71-126/2 1.0 1.75 6.5 8.5 9.75 Faint Faint Clear Faint clear A-71-126/3 4.0 7.5 9.0 9.5 9.75 10.0 12.25 Clear Clear Clear Clear Clear Clear Clear A-71-126/4 7.25 8.5 9.5 10.0 10.75 11.25 12.25 Clear Faint Clear Clear Clear Clear Clear A-71-126/5 Numerous indications faint to clear along the whole length, 14.5 clear.
5 A-88-ll 0.25 1.5 2.75 3.5 7.0 9.75 11.75 Faint Clear Clear Clear V Shape Faint Clear A-ll2-5 0.25 1.25 2.0 6.0 11.5 Lip Crack Clear Clear Clear Clear A-146-6 0.75 1.0 3.25-4.0 4.25 4.75 5.25 6.0 6.5 i
Clear Clear Clear Clear Clear' Faint Clear Clear A-146-8 1.ip Crack 0.25 1.0 4.0 4.25 6.'75 8.5 i
Clear Faint Faint Faint Faint Faint 15 2 5 10.25 11.5 i
Faint Faint f
I 11-11-23 1.0 1.25 1.5 2.5 Faint Clear Clear Clear 1
mWM l
21 3.5 Eddy Current Examination.
3.5.1 Results. Two types of eddy current (EC) probes were used in the examination of each tube segment. These were the differential or standard probe (Model No. A520LC) and the pencil probe (also kncun as the absolute probe). Both probes were obtained from ZETEC Corporation of Washington. An Eddy Scope Model EM 3300 from Aucomation Industries was used for displaying the signals, which were then recorded with a
~
Polaroid camera.
Test frequencies with the differential and pencil probes j
were 400 kHz and 350 kHz, respectively. The gain in the Eddy Scope was I
set such that a 100 percent through-wall defect in the ASME Section 11 standard produced a signal which covered one-third the width of the scope screen.
Tha differential probe was calibrated using an ASME Section 11 standard. No calibration was done for the pencil probe.
g.
Results of the EC examination of various tubes are listed in Table 2.
The location of each defect indicatica is given with respect to the top of the tube examined.
The circumferential position of a defect is indicated by degrees, following the standard practice (W-axis as 0*)
recommended by GPU-Nuclear.
3.5.2 Significant Observations. The results of EC examination are su=marized below:
(1) Defect indications in the roll transition region were obtained in tubes B-8-25, A-88-ll, A-112-5 and A-146-6.
(2) Defect indications were obtained in all tube segments, including those from the long-pull from below the upper tube sheet crevice region. Location of all indications from various tubes are listed in Table 2.
(3) Some defects indicated by the differential probe were not confirmed by the pencil probe, and vice versa.
However, in most cases indication of one probe was confirmed l y the other.
~
22 TABLE 2.
RESULTS OF EC EXAMINATION OF TUBES FROM TMI-1 STEAM GENERATORS A AND B USING DIFFERENTIAL A::D PENCIL PROBES D_efect Location
- DP PP Tube Number in.
in, degree Comment Note B-8-25 1.25,90-180 Large Signal Bracing roll transition 1.50, 320 Large Signal i
2.75, 180 Large Signal l
3.0 s90% Wall 3.5 s90% Wall 4.0 Surface Defect i
4.5 Small Signal 4.5, 180 Large Signal 5.0 Small Signal 4.75, 110 Large Signal 5.0, 90 Large Signal' 5.25, 110 Large Signal 5.75 Surface Defect 6.0 Surface Defect 6.75, 90 Large Signal 7.75, 60 Large Signal 9.25, 340 Small Signal 9.25 Surface Defect 9.75 Surface Defect
~~
1 23
)
TABLE 2.
(Continued)
Defect Location DP PP Tube Number in.
in, degree Comment Note i
B-11-23 0.25, 25 Large Signal Tube Stub (2.0 in) was examined after 0.75, 180 Large Signal cross sectioning the tube. No 1.0, 300 Large Signal indication in roll transition region.
L 10.25 Small Signal Remainder of the tube (long piece) af ter remo'-ing t'he thru-wall crack.
A-23-93 1.75 Small Signal 1.75,20-140 Large Sigual 2.5
%80% Wall 2.5,20-140 Large Signal A-71-126 2.75, NO Small Signal 3.0 Small Signal A-71-126 14.25 Possibly 0.D.
Ends flared to allow probes 24.25 Possibly 0.D.
A-71-126 33.25 Small Signal Ends flared to allow probes 33.25 Small Signal 36.75 Possibly 0.D.
A-71-126 49.25 Possibly 0.D.
Ends flared to allow probes A-71-126 52.75
<20% Wall 54.25, NO Small Signal MO
24 TABLE 2.
(Continued)
Defect Location DP PP
' ~ =
Tube Number in.
in, degrees Comment Note A-88-11 1.25, 270 Large Signal Bracing roll transition 5.0, 90 Large Signal 5.0 s100% Wall L.
A-112-5 1.25, 270 small Signal Bracing roll transition 3.25, 270 Large Signal 3.5 90% Wall 5.25, 270 Large Signal 6.25 90% Wall 6.25 90% Wall 6.50, 270 Large Signal 8.0 80% Wall 8.0, 270 Large Signal A-146-6 1.25, 5-260 Large Signal Bracing roll transition 4.0 Possibly 0.D.
8.25 s70% Wall 8.25, 5-260 Large Signal 10.25 s70% Wall 10.25, 180-290 Large Signal u
e 25 TABLE 2.
(Continued)
I a
Defect Location DP PP Tube Number in.
in, degrees Comment Note l
A-146-8 2.0 Medium Signal 2.0, 0-270 Medium Signal 3.75 N90% Wall 3.5, O Large Signal 6.0 s90% Wall 6.0, 350 Large Signal
.i Defect Location refers to the top end of each tube as 0.0 inch and degrees are referenced with respect to W-axis as 0*.
-t
-w
- e4 be==
I 4
w w
l l
4.0 RESULTS OY OTHER EXAMINATIONS 4.1 Tube B-8-25 Short-pull tube B-8-25 was examined using the following techniques:
+ -.
(1) Visual examination of U-bend slices (2) Visual examination of ID surface (3) Metallographic examination (4) SEM (Scanning electron microscope) and EDAX (energy dispersive X-ray analysis) examinations of fracture face 1.
(5) AES and ESCA examinations of fracture surface film.
[
Exanination results for tube B-8-25 are summarized in Table 3.
Also given in Table 3 are: a) the identification number of each specimen j-removed from the tube fer examination; b) loc.tcion of each specimen with respect to the top end and O' axis of the tube; c) type of any defect j
indication from NDEs, and d) type of examination performed on each specimen. Details of the examination results are given below.
Top end (specimen A) of tube B-8-25 containing the roll-i'-
transition area was slit into eight longitudinal slices.
This section had an EC indication at 1.25 inch location. Photographs of these slices (specimens Al-AS) are shown in Figure 16.
Specimen A4 broke into tuo pieces during slitting, and specimen A3 also showed a through-wall crack in handling.
Specimens A2, AS and A6 were bent into U-shape with ID in tension, all three specimens showed cracks with %90 percent wall penetra-tion. The cracks in specimens A2 through A6 were located at 1.25 inch and spanned from 45' to 270*.
Photemicrographs of the cross section of bent specimen A2 is shown in Figure 17.
A crack with 90 percent wall penetration is clearly visible in Figure 17.
The crack origin is at the ID surface of the tube.
All locations given hereia and af ter use top of the as-received tube as 0.0 inch reference, with inch fractions converted to nearest 0.25 inch.
M
)
y'
_7 TABLE 1 EXAMINATION,RESULTS OF TUBE B8-25 Specimen location Number Inches Degrees Type ofIndication Examination Result / Comment A (Al-A8) 0-2.25 EC 1.25 Slit and Bend No Crack at 04).75 At 0-2.25 0-45 OD Tension, Visual No Crack A2 0-2.25 45 90 ID Tension, Met.
1.25 IGC,90% Wall y Structure A3 0-235 90-135 SEM/EDAX 1.25 IGC,100% Wall;S 1.9%
AES/ESCA Fission Products and S (0.4%), Be (7.2%), Ag (03%)
Sulfkle l
A4 0-2.25 135 180 SEM (top) 1.25 IGC,100% Wall w
TEM (bottom)
No Striations A5 0-2.25 180-225 ID Tension, Visual 1.25 ICC,90% Wall A6 0 2.25 225-270 ID Tension, 1.25 ICC,90% Wall,S 53% Near ID SEM/EDAX A7 0 2.25 270-315 OD Tension,SEM No Crack A8 0-2.25 315-360 OD Tensior,, Visual No Crack B
2.25-3.25 0 180 EC 3.0, Visual Crack AES/ESCA liigh C(>50 a/o),S"(~l a/o),CI(<l afo), B (~3 afo)
No SOj Cl 3.25-12.0 0-180 EC Several Places ID Visual Tree Decoration C2 2.25 12.0 180-360 EC Several Places ID Visual Tree Decoration, Crack Appearance at 3.0,3.5,4.5 i
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P110TOCRAPil 0F AS-CUT SLICES Al TilROUGli A8 FROM TUBE B-8-25 i!
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INTERGRANULAR ATTACK FIGURE 17.
PHOTOMICROGRAPHS OF THE CROSS-SCCTION OF BENT SPECIMEN A2 FROM TUBE B-8-25
5
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A second IG penetration on the ID surface %40 mils above the main crack was also observed, Figure 17b. This IGA penetration is %50 percent through wall and the spread at the mid-wall is about 10 grains.
SEM photographs of the fractured surface of specimen A6 are shown in Figure 18.
The crack la completely intergranular and the wall penetra-tion is >90 percent. Cavities visible on the fractured surface in the mid-wall region indicate that the intergranular penetration was not limited to the transverse direction, but that some penetration also occurred in the longitudinal direction.
The fractured surface of specimen A6, at high magnification showed fluffy deposits on the grain faces, Figure 18.
The EDAX analysis of the fractured surface indicated the presence of sulfur. The concentra-tion of S on the surface ranged from 0.4 to 5.3 percent (as relative L.
X-ray intensity N atomic percent), depending upon the area analyzed.
I' Table 4 lists the EDAX results.
The fracture surface of the broken specimen A4 was descaled and then replicated for TEM examination. TEM photomicrographs of the i
replica are shown in Figure 19.
No fatigue striations were observed on the grain facets. This indicates that the failure of the tube was i
not due to corrosion fatigue but probably was the result of intergranular stress-corrosion cracking (IGC).
i
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Specimens A1, A7 and A8 were bent with OD in tension. None of these showed any crack on the OD or ID surface.
Specimen A7 when h.
examined with SEM showed only minor surface tears at the U-bend apex,
~
but no deep cracks, Figure 20.
The crack in specimen A at 1.25 inch was circumferential and limited to specimens A2 to A6 which covered 45' to 270' of the tube.
Specimen A3 was used for AES and ESCA analyses.
The surface of A3 that was analyzed contained intergranularly cracked area (% 80 per-cent of surface) and freshly fractured area (%20 percent of surface);
I the latter was produced from the mechanical removal of the uncracked ligament from the specimen.
The AES/ESCA instrument used in surface analyses was a Leybold-Heraeus *HS 10 System. The analytical chamber of the instrument operated 4w
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FLUFFY DEPOSITS FIGURE 18.
SDi PHOTOGRAPHS OF THE FRACTURED SURFACE OF SPECI'EN A6 FROM TUBE B-8-25
ge 4 7
J TABLE 4.
EDAX ANALYSIS OF FRACTURE SURFACE 0F SPECIMEN A6 FROM TUBE B-8-25 Relative X-Ray Intensity Tear Area In Fracture Close Fracture Fracture Close Remaining Ligament To Tear Center To I.D.
Cr 16.5 17.1 18.3 18.0 r,
Fe 10.1 7.2 7.3 4.0 I
l Ni 73.4 74.9 73.4 72.6 I
S 0.7 0.4 5.3 l
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TDi PHOTOMICROCFAPHS OF THE REPLICA 0F FRACTURE SURFACE OF SPECIMEN A4 FROM TUBE B-8-25 AFTER DESCALING E 4
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SEM PHOTOGRAPH OF THE APEX OF U-BEND OF SPECIMEN A7 FROM TUBE B-8-25
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'b at 5 x 10 to 1 x 10 torr vacuum. Auger spectra were produced with a U
j scanned electron beam of 5 kev, having a 5 pm spot size. Scanned areas L
on specimens for auger analysis ranged frcm 0.5 x 0.5 mm to 1 x 1 mm.
(!D Auger electrons emitted from a specimen were analyzed with a hemispherical photomultiplier detector. The Auger spectra of specimens were matched to y
standards given in " Auger Electron Spectroscopy Reference Manual"* for the j.
identification of elements.
ESCA spectra of specimens were produced with Mg-k, 1254 eV x-rays, from a gun operated at 12 kV and incident at N45* onto 1 cm2 area at p
sample location. Thus, the area of a specimen analyzed was that exposed to x-rays in the 1 cm region. If the surface area of the exposed specimen 2
was smaller than 1 cm, the x-ray photoelectrons for ESCA were produced from r--
t J the available surfacc, and the resulting signals were proportionately weaker.
_q The spectra of specimens were interpreted on the bases of standard binding and kinetic energies of electrons given in " Handbook of X-Ray Photoelectron Spectroscopy."**
The A3 surface was analyzed with AES in the as-received condition, i
and after sputtering-away 600, 900, 1200 and 15001 of the surface film.
The AES spectra was taken at several spots on the A3 surface, namely, in the IGC area at tube ID edge, center OD edge and front edge of the specimen.
The freshly fractured area of A3 also was analyzed. A quantitative esti-mation of elemental distribution over the entire A3 fractured surface was rj determined with ESCA af ter sputtering 0, 600 and 9001 of the surface film.
I The results of AES analysis are given in Table 5 and those of the ESCA J
analysis in Table 6.
c 1,y The AES detected a host of elements on the fracture surface as shown in Table 5.
The elements detected were C, 0, Fe, Ni, Cr, S, P, C1, B, Be, Zr and various fission products of uranium. The most predominant ele-ment on the surface was C, its concentration was 90 atom percent in the top 9C layer but dect:ased to 64.8 percent at 9001 depth, b
- G. E. McGuire, " Auger Electron Spectroscopy Reference Manual", Plenum L
Press, NY (1979).
- C. W. Wagner et al, (Eds.), "Handboost of X-Ray Photoelectron Spectroscopy" Perlain Elma Corp., Minn. (1979).
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.p+
11 TABLE 5.
AES ANALYSIS OF FRACTURE SUPJACE OF SPECIMEN A3 FROM TUBE B8-25 Depth Area on Sputtered Fracture Surface Elements Detected None IGC Center C, O, Cs, Y, Sn, La Fresh Fracture C
600A IGC Center C,K,B,Sb,P,Be IGC Edge C, K, Be, P, Y, S, B, Ag, Te Fresh Fracture C, Ni 900A IGC Edge C, Ag, Ca, S, P, Be, K, Ca 1200A IGC Edge C, Si, Be, S, Cl, Ar, Rh, Ag, O, Cr j i IGC OD Side C,Be,Ca,Ag IGC ID Side C, Si, B IGC Center C, Si, B, Ag, O
[
Fresh Fracture C, Ni, Cu, O u
1500A IGC Center C, S, Ru, Ag, Cs, O, Be, P O
IGC Edge C, Si, Be, P, Cl, Ag, Te, O, La b
~d e
12 TABLE 6.
ESCA ANALYSIS OF FRACTLTE SURFACE 0F SPECIMEN A3 FROM TUBE B8-25 l
i Depth Sputtered, Surface Composition, atomic percent A
Ni Fe Cr O
C S
Ag Be Cs P
Ru Cu' r,
None
~10
~90 600 3.0 1.7 1.I 11.1 75.8 4.6 900 3.4 2.3 1.5 11.8 64.8 0.4 0.3 7.2 0.4 0.5 0.9 6.6
'Cu from copper holder.
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13 The distribution of elements on the fracture surface was extremely nonuniform. Not only the distribution varied with the sputter-ing depth but also from one spot to the next, which might be enly a few micrometers away. Worth pointing out is the heavy concentration, 7.2 atom percent of 3e observed at 900 1 depth in ESCA analysis.
The total fracture surface area on A3 specimen was not large enough for very detailed ESCA analysis. Therefore, a second specimen, namely B, was used which consisted of multiple fracture surfaces stacked rogether, as shown in Figure 21.
The results of ESCA analysis are 4
summarized in Tables 7 and 8.
Note that both S and C1 were detected at N1 atom percent level uptothe2300Idepthanalyzed. Boron also was detected at this. depth in 3.3 atom percent concentration. Carbon as usual was high, 64.2 atom percentat30I,butlower48.9atompercentat23001 depth.
Note also theverylowconcentrationofoxygen,20.6atomparcentat30I,which decreased further with depth to 14.9 atom percent at 2300 I.
The chemical state of the elements, as determined from their respective binding energies in the ESCA spectra, are given in Table 8.
Only Cr and Fe are shown to be associated with oxygen. Sulfur was in its reduced state as sulfide, S", (probably as NiS) and C is thought to be in a form similar to graphite.
The ID surfaces of specimens C1 and C2 were only visually examined.
The whole surface was covered with dull-color surface film. Along the length of the. specimens several brown color decorations also were observed.
Each decoration had the appearance of a cree, i.e., it had a main trunk and some spreadout branches, see Figure 22.
The brown color decorations gave an appearance of some corrosion attack on the metal surface, underneath the surface film.
Some dark brown circumferential lines (wider than a hair strand) were observed at locations 3.0, 3.5 and 4.0 inch on the C2 specimen. These lines 1
gave an appearance of circumferential cracks, which may have been the cause of EC indications at these locations as reported in Table 2.
The specimen was not examined any further.
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PHOTOGRAPH OF SPECIMEN B FROM TUBE B-8-25 SHOWING MULTIPLE FRACTURE SURFACES STACKED TOGETHER FOR ESCA ANALYSIS
- O
R.
15
' TABLE 7.
ESCA ANALYSIS OF FRACTUR2 SURFACE
'r OF SPECDEN B FROM TUBE B8-25 l _.
~
Depth Sputtered, Surface Composition, atomic percent A
Ni Fe Cr O
C Cl S
B r'
30 8.9 2.I 2.8 20.6 64.2 0.8 0.6 150 18.1 3.2 3.6 16.8 58.3 0.6 0.7
~
400 15.4 2.8 5.6 18.4 55.6 1.5 0.7 1100 15.7 3.2 5.1 15.5 59.7 0.7 2300 21.3 3.8 6.1 14.9 48.9 0.6 1.1 3.3 t-9 G
tw e
=_____-_ _ _ __
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i TABLE 8.
ESCA BINDING ENERGIES AND STATES OF ELEE.NTS ON SPECIMEN B FRolf TUBE 38-25 Depth Sputtered, A
Ni Fe Cr C
Cl(a) b(a)
S 30 852.0 Ni 709.0 FeO 576.0 Cr2 3 285.0 C 162.0 S-2 O
150 852.0 Ni 709.0 FeO 576.0 Cr2 3 162.0 S-2 0
400 852.0 Ni 709.0 FeO 576.0 Cr2 3 198.0 162.0 S-2 0
r 1100 190.0 2300 198.0 190.0 162.0 S-2 (a) Too low intensty for high resolution.
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A TREE-LIKE BROWN DEPOSIT ON THE ID SURFACE OF TUBE B-8-25 9
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Short-pulltuieB-11-23wasexaminedusingthefollowing
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- N techniques:
U (1) Visu1P Examination of U-bend slices
-(2) Meta 11ographic examination (3) A23 sand ESCA examinations of fracture surface film s
3 (4) Wall thickness measurements.
t- ; 1 Ex m ination results are summarized in Table 9, using the same format as,in Table 3.
Detailsoftheyesultsaregivenbelow.
Visual examination of U-bend. slices from specimen F (i.e., F1 toF4)showedcracksatlocation'I.25 inch,180to360*. The specimen
.had an EC indication at 1.0 inch location. The crack penetretion was 70 q o 100 percent through wall. The matching specimen E (i.e. O o 180*)
t also showed 100 percent through wall crack, see micrograph in Figure 23.
AIintergranularlyattackedarea,N20percentthroughwall,wasobserved htheO'faceofspecimenf;theIGA_isshowninFigure24 A crack.in tube B-11-23 at location 2.5 inch, 90 to 270*, was s
through wall and visible t[the unaided eye. A photomicrograph of specimen A containing thesabove crack is shown in Figure 25.
The section of the crack shown 1s at'the 225* circumferatal location on the tube. The
~
track is clearly latergranular, with IGA spread at least 7 grains deep on either side of the crack.
IGA also was observed on the ID surface of the
~
tube, away'f romithe crack, +0.25 to - 0.25 inch, and also en the wall U 5* f ace) opposite to-the crack. The ICA in some places was 3 to 4 grains deep as shown in Figura 26.
The s'pecimen was examined after an oxalic acid etch,-and no IGA was found on the OD surface, either at the 45' location or
[
the 225* crack side location. This clearly indicates that the IGC initiated on the ID ' side of the cubi.
s N
The microstructure of specimen A after a phosphoric acid etch is s
shown in Figure 27.
The grain r,1::e ranged between 5 and 50 pm.
The average size of grains, when viewed at 100X, corresponded to ASTM No. 7 or 8.
Discrete
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TABLE 9.
EXAMINATION RESULTS OF TURE B11-23 Specimen 12> cation Number laches Degrees Type of Indication Examination Result /Comtr2nt A
2D 2.75 45-225 Radiograph, Visual Metauographic IGC 100% WaH,ID.lG A y Structure Discrete Carbide ppt Inter t Intra Granular B
7.07.5 0-360 None STEM Sent to MIT C
2 0-3.0 225-270 Radiograph, Visual AES/ESCA Crack Surface liigh C Some S l
D 6.5-7.0 0-360 None EPR Sensitization Specimen Mounted But Not Used E
0-2D 0 180 EC, Radiograph Wall Thickness OD348 min /0D365 max.
e*
y Siructuse IGC 100% Wall 80*, IGA 20% Wall 0*
F (F1-F4) 0-2.0 180 360 EC, Radiograph Wau Thickness OD361 min /0D377 max.
Bend Visual FI 0-2.0 180-225 1.25,1.50,~ 100% Wall F2 0-2.0 225-270 1.25,225-250 70% Wall F3 0-2.0 270-315 1.25,270 315 70% Wall l
F4 0-2.0 315-360 1.25,315-36090% Wau G
7.5 12.0 0-360 EC10D Corrosion Test Sent to 0RNL l
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PHOTOMICROGRAPH OF IGC IN SPECI.GN E FROM TUEE B-11-23 i
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PHOTOMICROGRAPH OF ICA IN SPECIMEN E FROM TU3E B-11-23.
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>.9u:
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FIGURE 25.
PHOTOMICROGRAPH OF SPECIMEN A F10M TUBE B-ll-23 SHOWING IGC AND SEVERE IGA 0: EITHER SIDE OF l
TE CRACK j
w--nprwyy-w--.-w-y.-y.9y y..
---,r,,p,,
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s u-
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i s, -.j ;
- tn-
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- 2 ' ';2g e
T' i
60X f
i
.a FIGURE 26.
PHOTOMICROGRAPH OF ICA ON THE ID SURFACE OF SPECIMEN A FROM TU3E B-11-23 M
bene
- 'e
24 A
f~
i 1-I
,m Oh.. _
r
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1.
j
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s,.,.. ws.$, k. Mf)sf. a,m%{W: e..'Q,.;f t..,,
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<-~
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y
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. 95 "y-P. y n., g)g,w. ~.',,es?.
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500X I i 1
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.s FIGURE 27.
PHOTOMICROGRAPH OF THE MICROSTRUCTURE OF SPECIMEN A FROM TUBE B-ll-23 I ^
u.,
C
a n
25 i
chromium carbide precipitates inside the grains and also on the grain l
boundaries are visible. The grain boundaries already affected by IGA a
were heavily attacked on etching with phosphoric acid.
[;
The renainder of the above crack contained in specimen C was analyzed by AES and ESCA. Spectra of the as-cut specimen showed C, 0
[
and Ni on the fracture surface. The surface was sputtered with 2 kev argonionbeam,andafterremoving20Iofthesurfacefilm,sulfurwas l
detected at one edge of the surface. Carbon on the surface was in very large contentration in comparison to the rest of the elements. Because
'{-
of the overwhelming concentration of carbon, a quantitative estimation L
of other elements was not attempedd.
The fracture surface ias further sputtered and analyzed at 50,
{
100 and 200 1 depths. With depth, the cc.ncentration of C and 0 decreased but that of Fe, Ni and Cr increased. The concentration of S inc.reased up r-ji to 50 I but decreased thereaf ter. The analysis was not carried beyond 2001 depth.
I i
Wall thickness measurement results are given in Table 10 for specimens E and F.
The maximum thickness measured was.0.0377 inch and q
the minimum 0.0348 inch. The thickness was generally 0.001 inch lower in the rolled section than in the unrolled tube.
y.
b 4.3 Tubes A-23-93 A-88-ll and A-ll2-5 f
Short-pull tubes A-23-93, A-88-11 and A-ll2-5 were examined
~
only visual 1y for defects in the roll transition region, by slitting the upper section (0-2.25 inch) of each tube into eight slices and bending
~
them into a U-shape. Wall thickness measurements, however, were taken of r-'
one tube. A-23-93.
Tube A-23-93 had an EC indication at location 1.75 inch
- 1 and tubes A-88-11 and A-112-5 at 1.25 inch.
Results of U-bend examinations of tubes A-23-93, A-88-11 and A-112-5 are summstized, respectively, in Tables 11, 12 and 13.
Wall thick-ness measurements of tube A-23-93 are given in Table 14
- 4p
~
- _ = -
(
26 i
TABLE 10.
WALL THICKNESS OF TU3E 311-23 I*
~
WallThickness inch
- Location, 45' 135*
225' 315' inches Position Position Position Position
~~
1/8 0.0348 04350 04368 04365
. {
l/4 04354 0.0351 0.0361 0.0368 tJ 3/8 0.0354 0.0355 04364 0.0367 1/2 0.0352 0.0353 0.0362 04363
,1 l, j 5/8 0.0352 0.0352 0.0364 04362 3/4 0.0356 0.0351 04364 0.0362
{;
7/8 0.0353 0.0350 0.0368 04362 1
04355 0.0350 0.0370 04365 i
11/8 0.0362 0.0360 0.0372 04370 l 'i l 1/4 0.0363 0.0359 0.0372 0.0372 l3/8 0.0364 0.0361 0.0372 0.0371
,.I 11/2 0.0362 0.0361 0.0373 0.0370 15/8 0.0362 0.0361 0.0377 04368 b
l3/4 04365 0.0360 0.0372 0.0370 17/8 0.0365 0.0359 0.0372 04370 u
3 9
?
9
>e.
e W
~
sonrt _
n
-]
r-1
-(.
t.
t.
J
_-J t _
TABLE 11.
EXAMINATION RESULTS OF TUBE A23-93 Specimen location Number Inches Degrees Type ofIndicasion Examinaston Result /Conunent l
A(Al A8) 3-2.5 EC 1.75,20-140 Wall Thickness OD357 min 10D37I max.
Radiograph Lip Crack Slit and Bend 1.5 Pits, No Crack Visible On As Cut llalves Visual Ai 0-2.5 6-45 No Crack A2 0-2.5 4540 1.75,609 ) Crack ~ 100% Wall y
A3 0-2.5 90-135 I.75,90-135 Crack ~100% Wall, Also his f
A4 0-2.5 135 180 1.75,135-140 Crack ~ 95% Wall A5 0-2.5 180 225 No Crack A6 0-7.5 225-270 No Crack,2.25 270 Pits j
A7 02.5 270-315 0.25,270-315 Lip Crack 100% Wall l
A8 0-2.5 315-360 No Crack
! l Reserved for B6W
- l Il 2.5-12 0360
~
t I
i l
0
-3 3
J i
t i
t -.
s J
J i
4 TABLE 12.
EXAMINATION RESULTS OF TURE A88-11 Specimen location Number inches Degrees Type of Indication Examination Result / Comment A (A l-A8) 0-2.5 EC, Radiograple Slit and Bemi Pits,at Several Places Visual At 02.5 045 0.25 Lip Crack A2 0-2.5 45s0 2.25,6090 Crack 90% Wall l
u A3 0-2.5 90 135 2.25,90-120 Crack 90% Wall i
om A4 023 135-180 1.25,130-180 Crack ~I00% Wall A5 0-2.5 180-225 1.25,180-200 Crack ~100% Wall A6 0-2.5 225 270 0.25 Lip Crack A7 0-2.5 270-315 No Crack A8 0-2.5 315 360 4
0.25 Lip Crack i
2.25,330-360 Crack 80% Wall 14 2.5 12.5 Unused i
4 i
E i
g g
s TABLE 13.
EXAMINATION RESULTS OF TUBE All2-5 Specimen location 1
Number Inches Degrees Type of Indication Examination Result / Comment A(AI A8) 0-2.5 EC, Radiograph She and Bend Visual AI 0-2.5 045 1.25,045 Crack ~100% Wall A2 0 2.5 45-90 1.25,4540 Crack 90% Wall,I.ip Crack I
w l
A3 02.5 90 135 No Crack:
A4 0-2.5 I35 180 0.251.ip Crack
{
A5 0-2.5 180-225 0.25 Lip Crack l
A6 02.5 225 270 0.25 Lip Crack I
A7 02.5 270-1,15 0.25 Lip Crack A8 02.5 315 360 1.0-1.25,315 360 ~100% Wall B
2.5-12.5 0360 Reserved for B&W i
t 1
i
30
(
i
TABI.E 14.
WALL THICKNESS OF TUBE a23-93 Wall Thickness. inch
- Location, 45*
135*
225*
315" I
inches Position Position Position Position L
2 1/8 0.0368 0.0361 0.0359 0.0357 I
1/4 0.0371 0.0360 0.0358 OD357
(
3/8 0.0370 0.0359 0.0357 0.0358 1/2 0.0359 0.0360 0.0358 0.0358 5/8 0.0359 0.0358 0.0358 0.0358 3/4 0.0360 0.0360 0.0358 0.0356 7/8 0.0361 0.0363 04357 OD358 1
0.0363 0.0362 0.0358 04357 11/8 0.0371 0.0365 0.0361 04362 11/4 0.0369 0.0362 0.0361 04365 l3/8 0.0366 0.0362 0.0362 OD368 11/2 0.0362 0.0362 04362 0.0369 15/8 0.0368 0.0362 0.0365 04368 t.
13/4 0.0362 0.0362 0.0370 0.0367 I7/8 0.0362 0.0361 0.0368 OD366 o
wmmm L.
~
~
^ '
~
J 31 Visual examination of tube A-23-93 revealed lip-cracks at location 0.25 inch, 270-315*, and a secon ! crack, nearly through wall, at location 1.75 inch,60-140'.
Some pits, probably. due to grain dropping.
l were also observed at 1.5 inch and 2.25 inch locations. Wall thickness of tube A-23-93 was me:h more uniform than tube B-11-23.
The maximum
~
thickness in tube A-23-93 was 0.0371 inch and the minimum was 0.0357 inch, E'
see Table 14.
~
[-
Three separate cracks were observed in tube A-88-11.
One was a lip-crack at location 0.25 inch, 315-45*, the second crack was at 1.25 inch, 130-200', and the third crack was at 2.25 inch, probably between 330 and 120', see Table 12.
g, Two cracks were observed in tube A-112-5.
One was a lip-crack at 0.25 inch,-135-315'.
The second crack was nearly through wall at 1.25 inch, 315-60', see Table 13.
i 4.4 Tube A-71-126 Long-pull taoe A-71-126 was exarined with the following techniques:
- i i
(1) Visual examination of U-bend slices l
(2) Visual examinatica of ID surface af ter descaling
}
(3) Meta 11ographic examination (4) Tensile test (5) Alloy composition f
( 6',
EFR sensitization test-
. r i
(7) AES and ESCA of the ID surface.
ti
("
4 Results of these examinations are summarized in Table 15 according to the format of Table 3.
Details of the results are given below.
f Specimens for visual examination of U-bend slices were taken
' from three different locations of the tube. The specimen X (X1 to X8) was from location 0-2.0 inch, speci=en Y (Y1 to Y4) from 2.0-4.0 inch, and specinen F from 50.5-58.5 inch.
it.us, specimen F was from the long-pull section that was well below the tube sheet crevice region.
w d
et-t y
---yee n ge-e, -
-,,MN g-y ag - s p eyg eo 3-y
- gqy
-n*g p +v a-gy 4-p y
y
+,, 9
TAllLE l'.
EXA}llNATION RESUI.TS OF Tulle A71-126 Specimen 1.ocation Number Inches Degrees Type of Indication fixamination Result /Conunent X (XI-X8) 0-2D Radiograph I.75 Slit and Bend Visual X1 0-2D 045 0.25 Lip Crack X2 0-2.0 4590 0.25 Lip Crack,1 D Pits X3 0-2 D 90-135 I D Pits X4 0-2.0 135 180 No Cracks XS 02.0 180-225 No Cracks X6 0-2D 225-270 Possible IGA X7 0 2.0 270 315 0.25 Rolled Metal X8 0 2.0 315-360 0.2$ Rolled Metal Y (Yi-Y4) 2D4D EC 3D Slit and llend Visual Yi 2 D4.0 0-90 No Cracks u
l i2 2.04 D 90-180 No Cracks Y3 2 D-4 D 180-270 No Cracks Y4 2D4.0 270-360 4
No Crack:
Z 4.0-13.0 0-360 Unused S
13D 25.75 0-360 Unused T
25.75-38.25 0-360 Ser.: to ORNL i
U 38.25-5 i D 0-360 Sent o ORNI.
A 59.0 60.0 0-180 None Alloy Composition 0.034%,C,15. 3% Cr 11 59.5 60.0 18d-360 None liPR Sensitia tion Activation Potential i10 mV (SCE)
C 52.0 52.5 180-360 Nonc ID AES/liSCA B (3.5%), Zr (0.3%), S (I D%), SOj Top /S" Ilot tom D
52.5 59.5 180-360 Radiograph Visual Descaled No Obvious Crack 11 51.0-52.0 180 360 Visual - Gouges None Unused F
$0.5-58.5 0180 Radiograph ID llend, Visual No Cracks (3X '".sual)
+
,~3
)
~
TABLE 15.
(Continued)
Specimen Incation Number inches Degrees Type of Indication Examination Resuk/Conunent G
60.0 68.25 0-360 Radk> graph Tensile Test, Slit Y!I53 KSI,UTS 101 KSI Visual No Other Cracks.Descaled il 68.25-68.5 0-360 Visual Gouges None Unused I
53.25-53.75 180-360 Visual - Pit:
Transverse Met.
Mechanical Indentatk>ns J
53.75 54.25 180-360 Visual - Pits longitudinal Met.
Mechanical Indentations t
m.
34 In spacinen X, a lip-crack was observed at 0.25 inch, 0-90*.
Some pits were also observed at 1.0 inch, 45-135*.
The nature of these pits, i.e., whether they were formed from mechanical damage of the tube or from grain dropping was not obvious. No other crack, beside the lip-crack was found in specimen X.
The radiographic indication at 1.75 inch was not confirmed as a crack with visual examination.
No cracks were found in specimen Y, which had an EC indication b
at 3.0 inch location.
Specimen F was a 8.0 inch long slice which was C
bent into a C-shape over a 4-inch diameter tube and then examined. No crack was found over its entire length.
The ID surface of specimen F, however, before bending was found to be heavily scored practically all over its length. A photograph of k
the descaled scored surface is shown in Figure 28.
The scoring marks were possibly responsible for the defect indications in radiographs, described in Section 3.3.
A general view of the ID surface of the tube section between 51.0 and 60.0 inches, before descaling is shown in Figure 29 Score marks can be seen on all quadrants of the section over its entire length.
The mechanical nature of the ID surface defects, as shown in Figures 28 and 29, is fairly obvious from the photomicrographs in Figures 30 and 31.
The photomicrograph is Figure 30 is a transverse cross section of specimen J, see Table 15 for their locations. The well defined trapez idal
. shape of the indentation in Figure 30, and the crushed grains on the surface at the defect site in Figure 31 are indicative of the mechanical penetration.
Specimen G, location 60.0-68.25 inch, was used for determining the mechanical properties of the tube uaterial. Two bullets (each 3.125 inch long) were inserted in the tube, one at either end, for proper gripping and defining the gage section. Thus the gage section in the specimen between the bullet heads was 2.0 inch. The length of the original 8.25 inch specimen after testing was 9.37 inch, i.e.,
the total elongation in the specimen was 1.12 inch.
Since no reference marks in
.J
_ = _ - _ _ _ _ _ _ _ _ _ _ _ _ _ -. _ - - - - -
- I
_ =_
35 i
l l
l 4
I
^
yp, u
' { Y"h.
_;q.l)t
- ^
h.; -
' !. S,;
i
(
[...,
~
s.
FIGURE 28.
PHOTOGRAPH OF THE DESCALED SPECIMEN F FR0M TUBE A-71-126 SHOWING HEAVY SCORING l
l l
t
/
. - - - - - - - - ~ - - - - - - - - - -
~~' '
' " ' ' ' ' ' ' ' ^ ~
e e
D 4
e e.
f 8
4 5
- LO E
I
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b Y
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e 4
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Z 7
wo 4
I 2
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r-m __ L _:.___ _ _
r-w-
4
37
. ~ - ;,- = :s-r-,,,.. n.-w
?.
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~-
).'C*u%g}fa
.3
&;t -
~ ;;&;=. ', g: M.Wyy;A
^
d k
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< ;;y
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's
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1
+
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+
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.;. j f,-p
/
5.,..-ldAP
' A f?' ) 's,'
ci *~,(fp ' -fix'
^
.Q xr..: *X'; *,'
{:f, ID 200X FIGURE 30.
PHOTOMICROGRAPH OF THE TRANSVERSE CROSS SECTION OF SPECIMEN I FROM TUBE A-71-126 9
m___._______
t 38 m
i L
, i r<
' ~ -jh ID p 3 F.,4,W',*#'
e 9
'g'
%=
k& ??Y.
L.1.M,W h,+E.Y4
.pql, y%
r et 1 :.
. '.s 7 ~:. 3:,;f., y;
. ;- 7: y
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. b I,~ *
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.a
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, t. c. '3'i {.], p 1
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- s.....s ~,_.._ _.. _
200X
?i i
FIGURE 31.
PHOTOMICROGRAPH OF THE I.ONCITUDINAL CROSS SECTION OF SPECIMEN J FROM TUBS A-71-126 czo
m 39 the gage section were made, the true percent elongation in the ma-terial could not be calculated.
The 0.2 percent offset (a clip gage used) yield strength of the material was determined as 52.8 kai from 3650 lb. load at yield and the ultimate tensile strength as 101 ksi from the 6990 lb. maximum load attained.
The above values are normal for fabricated Inconel 6008 tub ing.
Sp.cimen A, location 59.0-60.0 inch, was used for determining r-alloy composition By the X-ray fluoresence technique for all elements except C and N.
The C and N were determined with Leco instrument and N by a standard method. The composition of the specimen is given in Table 16.
The composition range with 0.034 percent carbon, and less than or equal to 0.01 percent S and P, is normal for an Inconel-6008 tubing.
The electrochemical potentiokinetic reactivation (EPR) test was done on specimen B to detect its susceptibility to polythionic acid attack. The EPR technique used was that described by Airey et al of LJ Wes tingho us e.*
The activation peak potential for the alloy was found to be 110 mV (SCE). After the test, the specimen surface was found to a
j be severely attacked in an intergranular mode. The high peak potential of 110 mV suggests, according to the Westinghouse paper, that the tube
[
is in a heat treated condition which makes it extremely susceptible to polythionic acid attack.
f The ID surface of specimen C, location 52.0-52.5 inch, was analyzed with ESCA.
Results are given in Tables 17 and 18.
The prime elements detected on the surface were Ni, Fe, Cr, 0, C, E. Zr and S.
The concentrations of Fe, Ni and Cr, as might be expected, increased with the sputtering depth, and those of C and 0 decreased. No definite trend emerged fer tha minor elements B, Zr and S.
It should be noted that the i_
0 on ID surface of the present specimens at %40 atom percent is about Laice as high as that observed on the fractured surface of specimen B from tube B-8-25, and conversely C at N20 atom percent is less than half l
of that on the above fractured surface.
G. P. Airey, et al, Journal of Metals, 33, 28 (1981).
- - " ~
cm
i 40 TABLE 16.
COMPOSITION OF TU3E A-71-126 ALLOY Element Wt. Percent Ni balance Cr 15.3 l,
Fe 9.6 Mn 0.36 Ti 0.21 f
Co 0.10 Cb
<0.10 r-Mo
<0.10 Cu
<0.10 Al
<0.10 i
Si Not determined properly (4.2) j P
0.01 S
<0.01 l
C 0.034 l
N 0.013 f
u l
b mm i
I y
l l
\\
l
~
i 1
e i
P 1
41 i
t t
TABLE 17.
ESCA ANALYSIS OF ID SURFACE OF E'
SPECUE.N C FROM TUBE A71-126 Depth Sputtered,
_Ni Fe Cr O
C d
Zr S
Surface Composition. atomic percent A
None 14.0 2.8 6.9 44.6 28.1 2.3 0.2 1.1 r"
30 18.3 4.1 8.4 43.3 21.4 3.5 0.3 0.6 630 24.1 5.1 10.7 41.1 14.6 3.2 0.3 1.0 1~-
1230 25.2 6.8 10.2 39.2 12.9 4.7 0.3 0.8 3630 28.9 8.0 11.7 39.8 10.4 0.0 0.4 0.8 l..
41 L
w t
4mm
t r-l 42 t
- TABLE 18.
ESCA BINDING ENERGIES AND STATES OF ELEMENTS ON SPECIMEN C FROM TUBE A71-126 Depth Sputtered, Ratio 1
A Ni Fe Cr C
S S-2 so4
=
/
'~
None 856.0 Ni(OH)2 711.0 FeOOH 577.0 Cr2 3 285.0 C 169.0 SO -2 o
0 4
I 30 856.0 Ni(OH)2 711.0 FeOOH 577.0 Cr2 3 285.0 C 169.0 SO -2 1,0 0
4
!62.0 S-2 I,
630 852.0 Ni 710.0 FeO 577.0 Cr2 3 285.0 C 169.0 SO -2 2.0 0
4
(
l62.0 S-2 1230 852.0 Ni 710.0 FeO 577.0 Cr,03 169.0 SO -2 2.0 4
162.0 S-2
(
l l
l 2430 852.0 Ni 710.0 FeO 577.0 Cr2 3 162.0 S-2
> io 0
i-855.0 NiO I...
3630 852.0 Ni 710.0 FeO 577.0 Cr;O3
> 10 I
855.0 NiO
.s l
I e
~
11,
e-r---
1 43 4.5 Tube A-146-6 Short-pull tube A-146-6 was enmined using the following techniques:
1~
(1) Visual and photographic examinations of the ID surface (2) Microstructure and microhardness measurements (3) EPR, sensitization test (4) Metallographic and SEM examinations (5) Electron microprobe analysis of a pit (6) XRD analysis of ID surface scrapings (7) AES, ESCA and SIMS analysis of ID surface.
a Results of various ensinations are summarized 1, Table 19 using the same format as in Table 3.
Details of various resu* s are presented below.
The whole segment of tube A-146-6 was slit into two halves, and their ID surfaces were examined visually and were photographed.. The. _ _ __.__
photographs are shown in Figure 32. The ID surface was dull in appear-ance and it was covered with thin deposits. Several spots were decorated with brown color irregular patterns; these appear as dark patterns in l
Figure 32. These decorations gave the impression that corrosion (or ICA)
)
had occurred at several points on the tube surface, and the corrosion product had seeped around them and produced these patterns.
r l
The patterns described here are similar to those shown in Figure 22 from.abe B-8-25, and described previously as tree decoration.
A minor difference between the two is that the lines forming the pattern in Figure 22 are narrcwer than the corresponding lines in Figure 32.
The reason for their appearance on the tube surface, however, is probably the same.
The microstructure examination and nicrohardness measurements i
were done on specimen 3, location 0.5-1.5 inch. The microstructure of l
1
'~
'~
j I
I I
e TABLE 19.
2XAMINATION RESULTS OF TUBE A146-6 i
i
{
i i
Specimen location i
Number Inches Degices Type of Indication Examination Result /Comnient f
i A
I 2 I.5 0 135 EC 1.25, Visual TEM A not Used, Substituted by B8-25 (A4) la 0.5-1.5 0 180 None y Structm e IMscrete Cashide pyt. No Continuous Netweek p liardness DPil Man.270/ Men.170 C
8.0-9.0 180 360 EC 8.25, Visual 360 longitudinal Met.
IGC 8.25,100% WaN Both Edges D
10.0 10.75 180 360 EC 10.5, Visual ID SEM, Met.
10.5 Pit + IGC,100% Wall 1
E 8.25-8.75 0 135 EC 8.5, Visual ID AES/ESCA 3100 A S (low) 0 (46%) C (8%) B (3%) Zr (0.2%)
l l'
i t
F2,3400 A S (0.7%) 0 (33%) C (19%) B (4%) Zr (0.3%)
r gF1 Fil) 0-5.5 225 360 Pits, Visual J
ID SIMS/ESCA Fi l,3500 A S (1.2%) o (4 I%) C (6%) B (8%) Zr (0.3%)
t (0.5 x II = 5.5)
Ni, NIO, Feo, c'2 3, S*
g 0
i G
5.5-6.5 180-360 Pits, Visual Microprobe lp S and Tiin Pit i
t 11 10.75 11.25 180-360 None EPR Sensitization Activation Potential 110 mV(SCE) 1 I
5.25-5.5 300-360 Pits, Visual XRD Unknc.wn Spincts. Nf3TIOS
{,'
(Part of Fil)
I I D 1.5 180-360 ODikposit Visual Transverse Met.
No Defect Under Ikposit,No lGA ID os OD (F3 Specimen)
- i j'
]
K 2.0-2.5 300-360 OD Deposit, Visual longitudinal Met.
No lkfect Under ikposit, No lGA ID or OD j
(F5 Specimen)
L 1.5-8.25 0-180 Tsee Deco.ation, Visual None Specimen Descale.i M
8.75 12.25 0-180 Tsee Decmation, Visual Mone Specimen Descafed
? '
i I
i I
1
45 w
k S.
w
,aP'*
i m,
i l.
FIGURE 32.
PHOTOGRAPHS OF ID SURFACES OF TWO HALVES OF TUBE A-146-6; A) 315' B) 225' C) 135*
~~ - AND, D) 45' FACE (SEE NEXT PAGE)
'c
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s a
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46 1,
the alley is shown in Figure 33 from three different sub-lcoations, i.e., rolled region, roll transition region, and the unrolled region.
There is no noticeable difference between the three microstructures.
In all three, the grain size is the same, and the carbide precipitates are discrets over grain boundar h s and inside grains. No continuous network of carbide is visible in Figure 33.
' 5 Microhardness values at 180* face of specimen B, taken at ap-proximately 1/8 inch intervals are shown in Figure 34.
Knoop diamond pyramid hardnese readings at any sublocation was taken every 4 mils starting at %2 mils from the ID edge of the tube. The highest values were in the rolled section of the tube (location numbers 1, 0.5 inch, to 5, 1.0 inch, in Figure 34).near the ID, the maximum was 270. In the roll transition region (location number 6, 1.1 ir.ch) the maximum value at ID was only 210. The maximum value below the roll transition region was
<200.
These values are considered normal for fabricated Inconel-6003 t
tubes, and the rolled region of the tube is not excessively cold worked.
~ ~
- An EPR test was done on specimen H from location 10.75-11.25
~
~
inch. The activation peak potential was obtained at 110 mV (SCE),
This value is the same as that obtained for specisen B of tube A-71-126.
According to the criterion used before, tube A-146-6 is extremely susceptible to IGA by polythionic acid.
Specimen C, location 8.0-9.0 inch, had a visible crack and f
also an EC indication at 8.25 inch. Brown color patterns were present on either side of the crack. Figure 35 is a photomicrograph of the
' j crack, which is intergranular and 100 percent through wall.
A defect associated with another brown color decoration was selected for SEM and metallographic examinations. Some white color y
deposits also were present at a few places over the decoration.
The area selected was specimen D from location 10.0-10.75 inch, which f
had an EC indication at 10.5 inch.
u A SEM photograph of an area including the white deposit is shown in Figure 36.
The surface appears cassty around the white deposit.
The specimen was then descaled and re-examined. Several areas on the surface were found to have pits and severe IGA. Pits appear to be in places where white deposits were-present on the surface before descaling of the specimen. One such pit is shown in Figure 37.
4
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FIGURE 33.
PHOTOMICROGRAPES OF THE MICROSTRUCTURE OF THPl?. ^;IFTERINT REGIONS 0F SPECIMEN 3 FROM TU3E A-146-6 9-MM-
48 i
280 260 Locanon 1 Location 5 Rsited Secuon Railed Secnon 240 220 -
200 I..
180 3,,
280 L'**'i'" 2 260 - Rolled Secten Locaten 6 Roll Tranunca
[
240
~
22a c.
200 i
180
{
3 160 3
280 E
l 260 L'*i*" 3 L'***" 7 g
Ro4ted Section Unrodied Secnon a
240 220 200 180 l
160 280
' l 260 Locetion 4 Locatw>n 8 i
Rouerf Secten Unrodied Secnon 240 m
~
200 -
180 0.004-
,0.004-i e
i i
i 3so 1
2 3
4 5
6 7
8 9
1 2
3 4
5 6
7 8
9 00 10 00 10
~'
PCSITION ACROSS THE TUBE WALL TUBE A 146-4 FIGURE 34 MICR0 HARDNESS VALUES AT 8 DIFFERENT SU3-I0 CATIONS ON SPECDIEN 3 FROM TU3E A-146-6
- = =
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- ' 4 w
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G NI AL
.... mm 100I l
FIGURE 35. PEOTOMICROGRAPH OF THROUGH WALL IGC IN SPECIMIN C FROM TUBE A-146-6 i
t.
5 er ie.
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. es 13SI FIGURE 36.
SEM PHOTOMICROGRAPH OF A 3R04'N SPOT AND 'GITE DEPOCIT ON THE ID SURFACE OF SPECIMEN D FROM TUBE A-146-6
~
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FIGURE 37.
SEM PEOTOGRAPH OF AN IGA PIT ON DESCnI.ED SPECIMEN D FROM TUBE A-146-6 l
F I-m aa
_T___
_'66 6
- "***~'#
'E
g,,,,
eme m eg a
- =a
- 44
=h b
J 52 The specimen was further cross sectioned very carefully (in the transverse' direction with respect to the tube axis) through one of the latge pits for metallographic examination. A photomicrograph of the cross sectioned pit is shown in Figure 38.
A through-wall IGC running from the bottom of the IGA pit is clearly visible in Figure 38.
Frem the examination of specimen C and specimen D, it is fairly certain that the crusty brown deposits and the white deposits on the ID surface are corrosion products. These were either released from the IGA
(
areas and solidified on the surface, or they were formed after the re-b leased corrosion product reacted with the tube surface.
A deposit similar to that shown in Figure 36 was cross sectioned C
and metallographically prepared for electron microprobe analysis. This was specimen G from location 5.5-6.5 inch, which had no EC defect i
indication. A back-scattered electron image of the ID surface of the specimen is shown in Figure 39.
A pit under the deposit is clearly q
visible.
J X-ray images of the speci=en for elements Ti, S, Cr, Ni and Fe also are shown in Figure 38. The deposit inside the pit appears Dg to be rich in Cr and Ti, but deplaced in Ni and Fe uth respect to che base metal. Sulfur is clearly present in all of the deposit. X-ray b
image of C1 was attempted, but no Cl was detected on the specimen.
Il
~
These readts again indicate that some corrosion product (s),
e.g., Fe++ released from the pit may have precipitated in the form of l
oxide (or hydrated oxide) giving rise to the brewn color patterns seen on the ID surface.
g I,
Some surface deposits, similar to that shown in Figure 36, were scraped from specimen I, locatioa 5.25-5.5 inch, for IRD analysis.
IRD patterns obtained indicated Fe, Ni,- Cr, some unknown spinels and i
N1 TiOS (pattern n.30-865). No sulfur compound =atched any of the
)
3 i
XRD patterns, i
ESCA results for quantitative analysis of the surface deposits of specimens F2, Fil and E are given, respectively, in Tables 20, 21 and 22.
The distribution of Fe, Ni and Cr on the three specimens at nearly the same sputtering depth were not significantly differene. In all three cases, Fe, Ni and Cr increased with the sputtering dep:h, as
~
might be expected.
4.s
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100I FIGURE 38.
PHOTOMICROGRAPH OF THE CROSS SECTION OF A PIT IN SPECIMEN D FROM TU3E A-146-6 G.
____.2J.=
ves CM6.
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w g.. ; -
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.a.. a wu,w,, x us...aws.x.au:z. w; w..~ w.. w w -,..=-. w,.
., : u
- .a u~: u a:.u iI t i FICIIRE 39.
BACK SCATTER ELECTRON UtACE AND X-RAY IMAGES OF ELEMENTS Ti, S Cr, Ni AND Fe OF A Pl1 I t' SPECIMEN G FROM TUBE A-146-6 i
i i
i 4
+
i r
53 l
TABLE 20.
ESCA ANALYSIS OF ID SURFACE OF SPECIMEN F2 FROM TUBE A146-6 Depth Sputtered, Surface Composition, atomic percent A
Ni Fe Cr O
C B
Zr S
~
fl None 5.5 3.7 4.1 43.3 39.5 3.8 0.2 r.
30 7.6 6.6 5.1 39.7 36.5 4.2 0.2 L
530 10.9 7.6 6.3 35.3 33.9 4.9 0.2 0.9 c,
(
1200 15.0 7.4 4.6 33.6 34.3 4.3 0.2 0.6 u
"~'2400 24.9 8.8 7.6 32.7 2b.3 3.2 0.2 0.3 3400 24.3 8.1 8.4 33.4 19.9 4.9 0.3 0.7 i
c, m.--
O f
N
- - - ~ ~ '
f
~.-..
)
~
i
', 6 i
I r
L TABLE 21 ESCA ANA*/*CIS OF ID SURFACE OF SPECDE! ill FROM TU3E A146-6 L
Depth Sputtered, Surface Composition, atomic percent A
Ni Fe Cr O
C B
Zr S
None 17.1 4.1 3.7 47.9 21.9 4.2 0.1 0.9 30 '
18.6 7.2 5..
45.1 15.4 7.2 0.2 1.2 530 22.0 67 6.0 45.2 12.4 6.4 0.2 1.0
~l130 25.2 8.5 6.7 39.8 11.5 6.6 0.2 1.5
~~
r--
i 2330 24.8 9.5 7.5 41.6
'1.1 7.4 0.2 0.9 t
3530 25.6 9.7 7.6 40.9 6.5 8.3 0.3 1.2 I
ye-
=e" I..
h
-e
-._n-
.-__._-.m-.
.-----~ -~~
~
- ~ ~ ~ ~ ~ ^ ~ ~ - ' ~
~
57 TABLE 22.
ESCA ANALYSIS OF I3 SURFACE OF SPECIMEN E FROM TUBE A146-6 Depth
~
Sputtered, Surface Composition. atomic percerit A
Ni Fe Cr O
C B
Zr S
l._
None 8.9 3.9 5.6 68.3 13.4 F'
350 12.5 6.5 6.0 57.8 17.3
)
600 13.9 4.0 6.9 58.9 16.3
!100 27.7 8.2 6.4 44.6 9.9 3.9 1600 28.3 8.7 7.3 43.5 7.7 4.3 2100 26.1 8.2 7.0 44.2 8.4 6.2 3100 22.0 8.6 12.1 46.3 7.7 3.2 0.2 1
O
__I__I_'_-__--.-..
~.. -. -
'S 58 AES/ESCA analyses were performed on the ID surface of three different specimens, namely, F2, Fil and E.
Locations of these in the above order were 0.5-1.0 inch, 5.0-5.5 inch and-8.25-8.75 inch. AES was used in conjunction with ESCA only to saot check the presence of i'
various elements on the surface. Therefore no separate results were o'otained via AES and none are reported here.
Oxygen on specimen F2 at 30 I depth was 39.7 atom persent and marginally decreased with sputtering to 33.4 atom percent at 34001 depth.
t, Similarly, oxygen or specimen Fil at 30 I vas 45.1 atom percent and 40.9 3530 I. On specimen E, oxygen was 57.8 atom percent at atom percent at
~
35 I and 46.3 atom percent at 3100 1. The order of oxygen concentration
[
on t!ie three specimens was the same, i.e., 30 to 60 atom percent. With sputtering, the total drop was minimal.
The C concentration on three specimens decreased noticeably with sputtering, see Tables 20 to 22.
The concentration dropped.from 36.5 to 19.9 for F2,15.4 to 6.5 for Fil and 17.3 to 7.7 atom percent for E.
Specimen F2 had nearly twice as much C on the surface as on Fil or E.
f' I
Boron concentration on all three specimens ranged between 3.2 and 8.3 atom percent. Similarly Zr was about 0.2 atom percent on the specimens.
r' Sulfur on specimen F2 fluctuated between 0.9 and 0.7 atom percent, and on specimen Fil between 1.5 and 0.9 atom percent. Sulfur r.
on specimen E was detected by AES at the depths investigated but the L.
concentration was not high enough (<0.1 stem percent) for detection by ESCA.
~
Binding energies of elements and their chemical states as
- j determined by ESCA analysis are given in Tables 23 to 25 for specimens F2, Fil and E, respectively. The top layer, O to %30 5, of the surface t-in each case contained hydrated forms of oxides of Fe and N1, i.e.,
Fe00H and Ni(OH)2 The most probable form of Cr on the surface was Cr 0 ;
23 however, the possibility of Cr00H cannot be ruled out..
With some sputtering, the prominent forms of Fe, Ni and Cr
~
oxides on the surface were determined to be Feo, N10 and Cr 0. Nickel 23 also was present in its elemental form.
h
~
. _ m.
59 l
TABLE 23.
ESCA BINDING ENERGIES AND STATES OF ELDfENTS CN SPECIMEN F2 FROM TUBE A146-6 Depth Sputtered, A
Ni Fe Cr I~ '
None 855.4 Ni(OH)2 710.8 FeOOH 576.4 Cr,0 or 3
CrOOH r,
30 855.4 Ni(OH)2 710.8 FeOOH.
576.4 Cr2 3 0
l-530 852.2 Ni 709.9 FeO 576.6 Cr2 3 O
854.8 NiO l
1200 852.2 Ni 854.8 NiO 709.9 FeO -
576.6 Cr2 3 0
1 2400 852.2 Ni 854.8 NiO 709.9 Feo 576.6 Cr2 3 O
3400 852.2 Ni 854.8 NiO 709.9 FeO 576.6 Cr2 3 0
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T
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60
.~
~
TABLE 24.
ESCA BINDING ENERGIES AND STATES OF ELIMENTS ON SPECIMEN Fil FROM TU3E All.6-6 Depth Sputtered, Ratio g
A Ni Fe Cr C
S S-2jso4
'p None-856 Ni(OH)2 714 517 Cr2 3 285 C 168 SO -2 o
0 4
2 30 856 Ni(OH)2 711 FeOOH 577 Cr2 3 285 C 162 S-2 g,4 0
r{
169 SO ~,-
4 530 852.2 Ni 710 FeO 577 Cr2 3 285 C 162 S-2 3
0 855.6 NiO 169 SO -2 4
.s 1130
' 852.3 Ni 710 FeO 577 Cr,0~3 285 C 162 S-2 4
855.0 NiO 169 SO -2 4
2330 852.3 Ni 710 FeO 577 Cr2 3 285 C 162 S-2
> 10 0
t-855.0 Ni 1
3530 852.3 Ni 710 FeO 577 Cr2 3 162 S-2 y to 0
859.0 NiO n
I
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61 T'
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1 TABLE 25.
ESCA BINDING ENERGIES AND STATES OF ELIF_NTS ON SPECIMEN E FROM TUBE A146-6 Depth Sputtered, A
Ni Fe Cr P
None 855.6 Ni(OH)2 711 FeOOH 576.6 Cr2 3 0
35 852.1 Ni(OH)2 711 FeOOH 576".6 Cr2 3 0
600 852.1 Ni 854.6 NiO 710 FeO 576.7 Cr2 3 0
1100 852.1 Ni 854.6 NiO 710 FeO 576.3 Cr2 3 0
I' 1600 852.1 Ni 854.6 NiO 710 FeO 576.1 Cr2 3 0
2100 852.1 Ni
- I 854.6 NiO 710 FeO 576.1 Cr2 3 0
3100 852.1 Ni
)'
854.6 NiO 710 FeO 576.1 Cr2 3 0
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62 The binding energy of C suggests that it is present as either graphitic carbon or bonded in long chain hydrocar5cus.
Tha S form on the top layer of speciran Fil was SO ", but 4
imeediately after some (30 I) sputtering sulfide, S", was also revealed.
With further sputtering, the ratio of S" to SO " progressively increased, 4
see Table 24. The S forms on specimens F2 and E are thought to be the same as on Fil.
Specimen F2 was examined by SIMS after the ESCA studies, i.e.,
after ion sputtering to 3600 I depth. The SIMS data were taken while sputtering with 19 ampere argon ion beam. The ien mass spectra were a
investigated from two areas on the surface. The areas used were (1) an apparent shallow pit and (2) a bright metallic spot. The principal ions detected were Cr, Fe, N1, Cr, A1, masses 69 and 70, with intermittent detection of 3 and S
- 2 Plots of ion intensity on a relative log scale versus approximate sputtering depth are shown in Figure 40 for the two areas
_. _ investigated._In the pitter. area, there was little. change in the intensities-----_ _
of mass 69, Fe, Ni, mass 70, Cr0 and Al up to the sputtered depth of %2um.
i, Sulfur, however, did go through a maximum at %1.5 um and then decreased.
In the metallic area, practically all ions showed a decreasing
(
[
trend with sputtering up to slum. Mass 70, however, went through a minimum at %0.5pm depth but then returned to the original value.
The masses 69 and 70 are ascribed to hydrocarbons with possible species of cyclopentana C N and its radical C Suc ydrocarbon 5 10 59 could be the source of carbon found in the ESCA spectra.
J All the examinations and their results described heretofore pertained to the investigation of the ID surface of tube A-146-6.
- However, two specimens, I and J, were metallographically examined with special m
attention te the CD surface. Specimen I was from location 5.25-5.5 inch i
and J from location 1.0-1.5 inch. These two were selected for examination because eney had deposits on the OD surface.
Metallographic examinations of the above two specimens showed no defects or IGA under the deposits or at any other locations in the cross sections examined.
e bA9
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63 V
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I I
I I
Pitted Area Metallic Ares (Analyzed Area 1 x 1 mm)
(Analyzed Area 1 x 1 mm)
~
Cr W
103 Mass 69 Fe Ni 2
~
~
Mass 69 8
Mass 70 u
Cr0 4,
2
_g 10 h,,
Al sa S
101
~
~
3; e Si
~
O 0.5 1.0 1.5 2
0 0.5 1.0 Sputtered Depth, um FIGURE 40. REI.ATIVE ION COUNT IN SIMS VERSUS APPROXIMATE SPUTTERED DEPTH CN THE ID SURFACE OF SPECIMEN F2 FROM TUBE A-146-6
~ ~ ^ ~ ~
~
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64 4.6 Tube A-146-8 Short-pull tube A-146-8 was exa=ined using the following techniques :
I (1) Visual and photographic examinations (2) Microstructure and microhardness measurements (3) EPR sensitization test (4) SEM and EDAX ernminations of ID surface and a fracture fact (5) Meta 11ographic examinations, r-Results of all ernminations are su=marized in Table 26 using the sa=e for=at as in Table 3.
Details of these results are presented below.
The whole seguent of tube A-146-8 was slit into two halves.
Their ID surfaces were examined visually and were photographed. The photographs are shown in Figure 41. The features described for tube A-146-6 also were observed on tube A-146-8, namely, dull color surface, deposits on surface, and brown decorations. Some scored areas also are visible in the photograph.
Specimen B from location 0.5-1.5 inch was used for amination of the microstructure and making microhardness measurements.
Photomicrographs of the etched speci=en from thre.e different regions of the tube, namely, rolled region, roll transition region, and the unrolled region are shown in Figure 42.
The grain size in all three regions is the same; similarly, the carbide decoration of grains and grain boundaries. No continuous networks of carbides were observed.
The microstructure of this tube is identical to that of tubes A-71-126
(?igure 31) and A-146-6 (?igure 33 ).
The microhardness measurements on speci=en 3 were done in the sane we.y as on tube A-146-6.
Results for tube A-146-8 are shown in l' igure 43.
The marimum value,DPH 241, was obtained on the ID surface in the rolled region, and the mini. n value, DPH 170, in the mid wall section u
of the roll transition region. These vclues again suggest that the tube was not excessively cold worked in any region.
i
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i TABLE 26.
EXAMINATION RESULTS OF TUBE A146-8 l
Specimen location i
Number inches Degrees Type ofIndication Examination.
Reside /Conunent
]
A 00.5 0-180 Radioseaph, Visual Longitudinal Met.
U Shape IGC i
B 0.51.5 0-180 Radiograph,1.0 p Structure Discrete inter- + intragrani:lar Carbide ppt p Ilardness No IGA on ID or OD,DPil 24l Max./l83 Min.
C 0 0.25 180-360 Visual U Shape Teansverse Met.
3 IGC,~ 100% Wall D
0.751.25 180-360 None EPR Sensitization Not Used, Substituted by L j
El 3.54.5 90180 EC 3.75, Tree Decoration longitudinal Met.
IGC,70% Wall, Microstructure As B j
i No ID or OD IGA E2 3.54.5 0-90 EC 3.75. Tree Decoralion SEM/EDAX IGC, Fluffy Deposit on Fractuse Face j
S and Ti
+
8 Ci F
3.5-4.25 180-360 EC 3.75. Tree Decoration Transverse Met.
No Defect Detected;No IGA ID or OD G
8.5-9.0 0180 Nonc longitudinal Met.
IGA 0.004 in. Deep /0.015 in. Wide at ID i
il 8.5-9.0 180-360 None Transverse Me1.
No Defect i
l 6.75 7.25 0-180 Visual ths SEM/EDAX Pits-lG A, ID Crust, S (7.8%), Ti (2.7%), Ca (0.1%)
l J
10.5 11.0 180-360 Visual Scratch!
locgitudheal Met.
No Defect
!I K
5.754.25 0180 VisualTree Decoration SIMS Not Used
,i L
0.254).75 180-360 None EPR Sensitization Activation Potential,125 mV (SCE)
I M
l.5-2.25 0-180 OD Deposit langitudinal Met.
No Ikfect Under Deposit, No IGA ID or OD l
I N
3.0-3.5 0-180 OD Deposit Transverse Met.
No Defect Under Deposit No IGA ID or OD i
1 1
i
66 r
b e
FIGURE 41.
PHOTOGRAPHS OF ID SURFACES OF TWO HALVES OF TUBE A-146-8; A) 45' B) 135' C) 225* AND, D) 315' (SEE NEXT PAGE)
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l 00 10 00 to PCSITION ACROSS THE TUSE WALL TU8E A 146 8 FIGURE 43.
MICRCliARDNESS VALUES AT 8 DIFFERENT SU3-LOCATIONS ON SPECIMEN 3 FROM TU3E A-146-8 (SEE TEXT) e-me-M4=W
>Wc@
4 gyp p ' w- * -
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@e m oaommgo.
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m ib 69 rgr The EPR sensitization test was done on specimen L from location
- 0. 25--0. 75 inch. The activation peak potential for this tube was 12' mV(SCE), which indicates a very high susceptibility to IGA by poly-thionic acid.
This value is not significantly different from the 110 mV value obtained for other tubes.
A defect with EC indication at 3.75 inch as selected for
]
SEM/EDAX and metallographic eminations. A circumferential crack at 3.75 inch location was visible to the unaided eyes. Some brown color decorations around the crack also were' present. Two specimens containing the defect were prepared from location 3.5-4.5 inch, specisan El (90-180 degree) for metallographic examination, and specimen E2 (0-90 demee) for Is SEM/EDAX analysis.
..]
The general appearance of the ID surface of the tube in the
]
brown' decoration area is shown in the SEM photograph in Ftgure 44.
The l'
surface is rough and is covered with granular and flaky deposits. Another 7-.
spot from a similar area showed crusty deposits on the surface, as shown
('
in the SEM photograph in Figure 45.
EDAX analysis of the spot in Figure 45 detected only Ni, Cr, Fe, T1 and S on the surface. The S was present in about C.2 weight percent concentration. Approximate concentrations of other elements on l
the spot in atom percent were: Ni-44; Cr-25; Fe-20; and T1-0.9.
In relation to the composition of base metal, i.e., Inconel 600* the spot p
appears to os rich in Fe and Cr but depleted in Ni.
Iron in the form of oxide may have produced the broun coloration on t' 4 surface.
m.
The apparent crack in specimen E2 was mechanically pulled apart, and the fracture surface was examined in the SEM. A SEM photograph of
~
the fractured surfcce in Figure 46 shows the intergranular nature of the crack. A photomicrograph of the same crack present in metallographic 1'
specimen El is shown in Figure 47. The crack is intergranular and p
penetration is %70 percent through wall. No IGA was noticed on the ID L
or CD surface of the tube in the vicinity of the crack.
A transverse cross section of the tube, specimen F 3.5-4.25 inch, 180-360 degree, showed no IGA attack on the ID or OD when examined metallographically.
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FIGURE 44 SDi PHOTOGRAPH OF A 3 ROW DECORATION ON THE ID SL3 FACE OF SPECIMEN E2 FROM TU3E A-146-8 4
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SDi PHOTOGRAPH OF A CRUSTY DEPOSIT IN A 3ROWN SPOT ON THE ID SURFACE OF SPICIMEN El FROM TU3E A-146-8 9
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FROM nile A-146-8SEM PHOTOGRAPH OF THE FR j
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PF.OTOMICRCCRAPH OF AN IGC IN SPECIMEN E1 FROM TUBE A-146-8 6
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74 Specimen I was taken from location 6.75-7.25 inch for another SEM and EDAZ examination. There was no defect indication from NDE for this location, but a shallew pit was visi51e on the ID surface. A SEM photograph of the pit is shown in Figure 48. Eatrustation around the i
pit is similar to that shown in Figure 45.
EDAX analysis of the surface found, in approximate atom percent, elements:
Ni-44, Cr-41, Fe-12, Ti-0.8, S-0. 8, and Si and Ca in small amounts. Another analysis of the inside surface of the pit found the deposits to be rich in Cr (76 percent) and low in Fe (~3 percent) and j
Ni (~17 percent). Other elements Ti, S, Ca an'd Si were also present in small amounts.
At one area inside the pit very high sulfur (7.8 percent) was detected, Ca (0.1 percent) and Ti (2.7 percent) also were present in the area. The descaled pit is shown in Figure 49. Intergranular attack is clearly visible i~n the SEM photograph.
Specimen G, location 8.5-9.0 inch, with no apparent defect on
(_
the ID surface and no NDE indication was examined metallographically.
IGA was observed on the ID surface of the tube,,as shown in Figure 50..
The IGA is approximately 0.004 inch deep and 0.015 inch wide at the ID surface.
A lip-crack from location 0-0.5 inch was metallographically examined. Two specimens A and C from the 0-0.5 inch location were j
c.
prepared for the examination. Speci=en A, 0-180 degree, was examined e
in longitudinal cross section, whereas specimen C, 180-360 degrees, was examined in transverse cross section with respect to the tube axis.
t
. I l
Micrographs of specimens A and C are shown in Figures 51 and l
52, respectively. In specimen A, the tube wall separated at the main crack while preparing the metallographic mount, the separated wall is j
visible in Figure 51. A second crack which appears to be a major branch j
of the main crack also is nearly through wall. The transverse section in specimen C showed three different unconnected cracks. One such crack i
only is shown in Figure 52; the other cracks were similar in nature.
Two specimens H and J from locations 8.5-9.0 inch and 10.5-11.0 inch showed no IGA attack on any surface ID or OD when examined =etal-lographically. There were no NDE defect indicacica at the above locations.
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FIGURE 48.
SEM PEOTOGRAPH OF A SHALL0t? PIT ON THE ID SURFACE OF SPECIMEN I TROM TUBE A-146-8 i
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l FIGURE 49.
SEM ?HOTOGRAPH OF A DESCALED PIT ON THE ID SLTFACE OF SPECDE.N I FROM THE TU3E A-146-8
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FIGURE 50. ?HOTCMICROGRAPH OF AN ICA CN SPECIMEN G FROM TUBE A-146-8
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FIGURE 51.
PEOTOMICROGRAPH OF AN IGC IN LONGITJDINAL CROSS SECTION OF SPECDIEN A FROM TJ3E A-146-8 I
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PECTOMICROGRAPH OF AN IGC IN T?ANSVERSE CROSS SECTION OF SPECIMEN C FROM TU3E A-146-8
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Two more specimens, M and N, from locations 1.5-2.25 inch and 3.0-3.5 inch showed no defects on either the ID or OD surface in e.etal-
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lographic avaminations. These specimens were particularly selected for CD examination since deposits were present on the CD surface. A similar I
resuir was obtained for tube A-146-6.
It is reasona51e to conclude that e
there are no defects on the JD side of tube A-146-6 or A-146-8.
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5.0 RESULTS OF Y-RAY ISOTOPIC ANALYSIS Five wipe samples from GPU-Nuclear were received for Y-ray isotopic analysis. Results of the analysis of each wipe sample are
- {_
summarized in Table 27.
Fission products detected on various samples 241 57 125 106 110 134 54 60 60 were Am Co, Sb
, Ru
, Ag
, Cs
, Mn and Co The Co
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was the main source of Y-rays in these samples. The next most prevalent 106 241 134 L
isotope was Ru Americium and Cs were detected on only one wipe sample which was from OTSG-B.
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TABLE 27.
CAHMA RAY ISOTOPIC ANALYSIS RESULTS I
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l ISOTOPE PERCENT l.
SAMPLE IDENTIFICATION W
gg AU AL BU BL R71T126 R149T15 Batch #66 R75T3 Batch #66 Isotope Sample #31 Sample #6 Sample #20 Sample #13 Sample #28 241 Am 0.1 n
i 57 i
Co 0.2 0.3 0.2 0.2 0.2 Sb 3.1 3.5 3.5 0.4 106 Ru 5.9 7.4 4.4 8.4 4.9 l
110 Ag 0.2 0.7 0.3 0.8 0.5 Cs 0.2 Ha 1.3 1.3 1.6 1.0 0.9 1
60 Co 89.3 86.8 93.5 86.1 92.8 I'
Notes:
(1) Lfhole sample analyzed; (2) %1/5th sample analyzed; (3) %1/5th sample analyzed; (4) llhole sample analyzed; (5) Sl/Sth sample analyzed 1
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6.0 DISCUSSION The results of various examinations are discussed here. The aspects considered in the discussion are a) nature of defect, b) defect location vs. NDE, c) physical and chemical properties of OTSG tubes, d) surface film composition and finally,e) probable cause of attack.
Nature of Defects Tubes A-146-6 and A-146-8 had typical dryout deposi;6 on their OD surfaces. Four specimens, two from each tube, having these deposits, were metallographically examined in longitudinal and transverse cross s ect;.on.
The two specimens from tube A-146-6 were from just below the roll transition region, whereas those from tube A-146-8 were from the icwer part of the tube segment. No IGA or other defects were observed on these specimens.
The OD surfaces of the above two tubes also were visually examined after brushing off the deposits at a few places. The surface underneath
)
the deposic had a metallic luster, but no corrusion attack or significant etching was observed. The OD surfaces of these tubes were not examined in the SEM. However, on the basis of visual and metallographic results it is assumed that no OD defects exist under dryout deposits on tubes A-146-6 and A-146-8.
Since tubes A-146-6 and A-146-8 had typical dryout marks, it is l
likely that other tubes also do not have CD defects.
l From the extensive metallurgical and SEM examinations of vari 7ur l
l specimens frem different tubes, it is fairly obvious that the main mode of attack in the tubes is IGA.
Further, the attack initiated on the ID surface of tubes. This attack produced three different kinds of defect geometry in the tube walls: a) ICA-islands, with grains retained, b) ICA-pics and, i
i c) stress assisted deep intergranular penetrations which may be called intergranular stress corrosion'eracks (IGSCC).
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2 One procinent IGA island 0.004 inch deep and 0.015 inch wide on the ID surface of tube A-146-8 is shown in Figure 50.
But some minor IGA areas were also seen in the SEM on a specimen from tube A-146-6.
It is very likely that similar other islands are present on other tubes, particularly under ID deposits.
+
IGA-pits ranged in size from a f ew grains deep and a few grains wide, as in Figure 37 to so.014 inch deep as in Figure 38.
IGA-pits are a result of grain dropping from the heavily attacked ICA-islands. Grains p
from attacked areas dropped off either because the grain boundaries were
[.
heavily attacked and no cementing bond existed between the grains, or because of the force of voluminous corrosion products generated at the grain boundaries, or both. In some cases the voluminous corrosion product filled the entire pit; an example of this is in Figure 39.
The cracks, i.e., IGSCC, were circumferential and spanned from l
1/8 to 3/4 of the circumference of a tube. The IGSCC penetration in various tube sections examined ranged between 20 and 100 percent through wall. Some of the cracks were vide open, e.g.,
in tube B-11-23, whereas others had to be opened up mechanically as in the case of 3-8-25.
f The IGSCC was produced in areas of IGA where stresses were high locally. A striking example of this is shown in Figure 38, in which the origin of the crack is clearly at the base of the pit.
The pit in this case apparently had acted as a stress concentrator in the tube, and subsequently, high stresses opened the attack grain boundaries thes forming the crack.
Another exanple of IGA leading to IGSCC is the crack in tube B-ll-23, Figure 25.
The IGA was found three to fcur grains deep on the ID surface of the tube, %0.1 inch on either side of the main crack, Figure 26.
Most of the cracks examined had seme branching. The IGA also was present along sides of crack walls, but the extent of IGA va,ried considerably I
from one crack to the next. Crack wall ICA was only one to two grains deep in some cases, see Figure 47, but seven to ten grains deep in others, j
Figure 25.
Meandering of the crack or IGA in a plane perpendicular to the l
fracture surface is fairly evident in Figure 19.
The deep cavities visible l
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in the mid wall are indicative of the spiraling. A similar conclusion can be drawn from Figure 52, which shows branched cracks present on a transverse section of tube A-146-8.
The three different kinds of defect geocatries, mentioned l
earlier, mainly reflect different degrees of IGA at localized areas.
Several factors related to mechanical, environmental and metallurgical conditions, e.g., localized stress, uneven distribution of aggressive chemicals (e.g., sulfur oxyanions and oxygen) on the tube surface, localized differences in degree of sensiti=ation, uneven oxide film, surf ace deposits, inclusions, and manufacturing defects, etc., may have been responsible for the different geometries. Considerable amount of experimental work will be required to pin-point the actual cause.
There is, however, some indication in the literature that the
{
rate of IGA, in the case of polythionic acid corrosion of sensitized Type 304, is strongly stress dependent. The rate of IGA on sensitized Type 304 is substantially low in the absence of stress, but very high in the presence of applied stress. The actual rates were not given by the authors, but the unstressed specimens showed only minor IGA when they vere exposed for 11 days in polythionic acid; on the other hand, the specimens stressed to 95 percent of their yield failed in'a few hours.
If a similar condition is believed to apply to IGA in sensitized Inconel 6003 tubes, the local variation in residual stresses could have been one principal cause of the different degree of attack observed in various parts of the same tube. But contributions from other fact l
such as oxygen distribution, etc., cannot be completely ignored.
The possibility of tube failure due to corrosion fatigue was ruled out frem the results of the TEM examination. No fatigue striations were observed on grain faces of the fracture examined, Figure 19.
Some mechanical defects also were found on the ID surface of several tubes. However, these were considered to be the results of either
- I. Matsushina, " Electrochemical Charatteristics of Polythionic Acid Cctrosion Cracking," Proceedings of the 6tn International Congress on Yecallic Corrosion, Sydney, Australia (1975).
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the tube pulling operation or were manufacturing defects. The heavily scored ID surface of tube A-71-126 on metallographic examination showed mechanical indentations on the wall. The presence of deposits inside indentations suggest that the defects were caused by tube manufacturing processes and the deposits formed af ter the exposure of tubes to aqueous environment in the OTSG.
i ^
Physical and Chemical Properties of Tubes. The chemical compo-sition, tensile properties, microhardness, grain size, and the micro-structure with respect to carbide precipitates of tubes are those of a normal cold drawn stress relieved Inconel 6003 tube. The grain si:e
'~
(ASIM No. 7 - No. 8) was uniform at different locations examined for several tubes. No continuous network of carbides was observed in any l
tube, thus, indicating no severe sensitization. However, the EPR test showed that the tubes are in a heat treated condition which is very i
i susceptible to polythionic acid intergranular attack. The EPR peak potentials of tubes were between 110 and 125 mV (SCE). During the EPR test, tubes were, in fact, heavily attacked intergranularly.
_=.
Surface Film Cemoosition f
The major foreign elements detected on the fracture surface of any specimen were C, S and C1, not considering oxygen. The distribution of S on the. surface was quite non-uniform, as shown by all the microanalytical techniques, i.e., EDAX, AES and ESCA. The concentration ranged trom practically nothing (i.e., below detection limic) to almost 8 atom percent.
Chlorine was detected only by ESCA at si atom percent level up to 23001 l
depth analyzed. Sulfur in the attacked area was found all the way down to the base metal as indicated by X-ray images of a sha11cw pit, see Figure 39.
No chlorine was detected by this technique.
The concentration of carbon on the fracture surface was very high j
>50 atem percent and that of oxygen comparatively low, 18 atom percent.
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5 Chemical statas of the major elements were Ni as elemental N1 or tied to sulfur, Fe as Fe0 and Cr as Cr 0. The S was in its reduced 23
~2 state as S The very low level of oxygen on the fracture surface agrees with the reduced states of Ni and S.
Carbon was as in graphitic carbon j ^
or long-chain hydrocarbon.
Major constituents of the ID surface film on tube A-146-6 were Ni, Fe, Cr, O and C.
Small amounts of B, S and Zr also were present.
i The same constituents also were found at location 52.0 inch on the long-pull tube A-71-126.
Nominal concentrations of the elements.as determined by ESCA up to a depth of 3500 I on both tubes were (in atom percent)
Ni 25 Fe 8, Cr 9, 3 3, S 1, and Zr 0.2.
No significant difference was observed in element concentrations because of the location of specimens with respect to the tube sheet. Sulfur was nominally at 1 atom percent.
SIMS analysis of one specimen showed that S on the ID surface was l
persistent up to at least 1.5 gm depth.
Thetopmostlayer(%1100I)oftheIDsurfacefilmwassome-what exidized (e.g., S as 50 "; Ni as NiO) as indicated by ESCA. But 4
thereaf ter, reduced S as S" was the prevalent form. Nickel, Fe and Cr at this level were as Ni and NiO, Fe0 and Cr 0.'
23 These analyses show that there is no significant difference between the states of elements on the fracture surface and the lower
[
layers of the ID surface. The one acticeable difference is that C on the fracture surface is at twice the concentration of that on the ID surface. The oxygen level is also two to thraa ti=es higher on the ID surface, but this could be simply because the ID surface was exposed to ambient environment for a long time, whereas the IGA-affected areas were protected by corrosion products.
The presence of high carbon in the ID surface film and in the fractured surface film is disconcerting. The SIMS analysis of ID surface, Figure 40, showed that C is persistent devn to %2.0 pm depth analyzed.
The fracture surface film was analyzed with AES/ESCA to only %2300 I (0.23 um) depth, but it is likely that C was present at greater depths.
In both cases, the che=ical form of C determined by ESCA was the same, w
._ - - - - ~
6 the binding enetgy for C atoms was as in graphitic-carbon or long
, chain hydrocarbons. It is reascuable.to cruelude that the C was deposited on both the surfaces from the same source.
The tube specimens for surface analyses was sectioned using a j'~
hand operated javaler's saw (hack saw). No lubricants were used in the operation. Sectioned specimens were stored immediately in clear plastic vials. The possibility of specimen contamination with carbon during j
sectioning and handling operations was therefore low.
However, minor contamination of specimens from air exposure and also inside the vacuum chamber (from residual vacuum pump oil vapors) of instruments is a definite possibility. Carbon from such contamination is often detected on specimens in AES/ESCA analyses. But this type of contamination is usually limited to the uppermost layer (50 to 100 A) of the surface film on specimens, if the film is non-porous. The contamina-tion is easily removed by argon ion sputtering.
During the AES/ESCA analyses of OTSG tubes, the specimen holder, which was made of copper, was checked in a few instances for surface contamination. Carbon was detected on the copper holder prior to any
~
e argon ion sputtering, but af ter about 50 A of sputtering, C was virtually all removed.
In the case of specimens with porous surface film, which probably was the case with OTSG tubes, the C contamination could have been deeper, and therefore, not easily cleaned off by argon ion sputtering. It is likely, therefore, that the total C measured on the tube surfaces had some contribution frem contamination in the instrument. The exact contribution l
to C analyzed is not determinable, but it is considered to be a small fraction i'
of the total.
The Preliminary Failure Analysis Report issued by GPU-N indicates l
that some oil may have been accidently introduced in the reactor coolant during the plant layup in March, 1979. It is likely that some oil migrated i
i to the steam generators, adhered on the tube walls and permeated the surface film. The chemical form of C in the oil would easily account for that determined by ESCA on various tube specimens.
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If the oil was not removed from the OTSG system, it is likely that the oil survived the hot functional and it was present in the
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system during the subsequent layup. If the cracking of tubes occurred (either aefore or after the hot functional) when the oil was present in the system, indeed carbon could have deposited on the fracture surf aces.
The fracture surfaces (Figure 21) analyzed by AES/ESCA were from a crack which had penetrated s90 percent of the tube wall. Therefore, it can be presumed that the crack walls were sufficiently open, under the cens11e i
stress present during the cold layup, to allow entry of oil into the crack.
Defect Location vs NDE Defects confirmed by destructive examination of numerous specimens from different tubes always corresponded to EC observations, except in two In tube A-146-6 at location 6.0 inch, a small pit was observed, cases.
Figure 39, which was not detected by EC at "attelle, and the GPU-Nuclear EC data file also does not show any indication for this position. Similarly,
_ _. _. _. _..no EC_ indications were given by either Battelle or GPU-Nuclear for the IGA defect, Figure 50, in tube A-146-8 at location 8.75 inch.
e l
The first undetected defect, i.e.,
the pit was rather small, 0.003 inch in diameter and 0.001 inch deep, but the IGA was 10 percent through wall. Sizes of the above defects are al= cst belew the detection limit of some of the EC probes.
Defect indications obtained frem radiographs were not always con-firmed as IGSCC or IGA. These indications we,re most probably from the
~
scoring of ID surface during tube pulling operation. Radiographs also were not able to detect very tight cracks.
A majority of confirned defects in tubes were located in the 4
roll transition area. The main reason for the preponderance of cracks in that area appears to be high concentration of stress, which assisted in propagation of IGA as discussed earlier.
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on the tubes is primarily in the form of sulfide (NiS or Ni S ).
The 23 sulfur compounds present in the OTSGs were reduced to either sulfur or sulfide at high temperature in the presence of hydrogen during the hot-3 functional. The reduced compounds ultimately reacted with the tube surface producing the sulfide film.
(3) Following the hot-functional, the OTSGs were partly drained for plant maintenance. The water level was kept near the upper tube sheet, but fluctuated by several inches be-tween September and November of 1981. The atmosphere inside the channel head during'this period was primarily air.
It is believed that the nickel sulfide reacted with the oxygenated water and produced the polythionic acid (e.g., 8NiS + 2H O + 110 = 4N1 02 3 + 2H S 0 ), by a mechanism similar 2
2 246 to that= proposed originally by Brophy* and later confirmed by Ahmad et al.*
The polythionic acid attacked the susceptible Inconel 6003 and produced the IGA.
The attack was primarily limited to those regions of tubes
^
where the stress' concentration was high and the oxygen was readily available, j ~
The above two conditions were adequately present at the water / air interface
{'
in the upper tube 'heet region, particularly at the rolled section of tubes.
+
This explains the reponderance of defects in tubes in the upper tube f
sheet region.
(4) Several. elements, primarily fission products and carbon, beside sulfur were detected on the tube surface as well as on fracture sur-faces. Whether these elements played any role in the attack mechanism can not be said with certainty. However, in view of the strong attack by poly-chionic acid, the role of other elements is considered to be nominal, if any.
- S. Ahmad et al., Corrosion. 38, 347 (1982).
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7.0 CONCLUSION
S Our general conclusions regarding the failure of Inconel 6008 tubes in tha OTSG A and 3 of TMI-1, based on examination results are as follows:
(1) Inconel 600* tubes failed by intergranular cracking (IGC)
(2) The cracks initiated on the inside surface of tubes and propagated outward.
f, (3) Ths cracks are characterized by severe inter-granular attack (IGA) on either side of the t'
i*
Crack (4) Some small areas on the inside sarface have IGA % 5 mils deep But with no cracks associated with them.
(5) The cracks and the IGA have been found in the entire length of the short-pull section of tubes.
(6) Whether the attack (IGA or IGC) extends beyond the short-pull length has not been fully evaluated (7) There was a preponderance of cracks in the roll transition region of tubes, high stress concentra-tion in that part of the OTSG appears ce be responsible (8) The most probable species responsible for the intergranular attack are the derivatives of sulfur (such as polythionic acid and thiosulfate) which was found in significant concentration on the fracture surface (9) There was no defect observed on the OD side of tuhes under dryout deposits
I I
2 (10) Some fission products, carbon and beryllium also were found on the fracture surface and on the inside surface of tubes; their role, r
if any, on the tube degradation process (es)
J, is not discernible at present.
(11) rhe attack on tubes nest probably occurred during the layup following the hot-functional.
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00 10 b0 lb POSIT!CN ACROSS THE TU8E WALL TUBE A 146 8 FIGURE 43.
MICR0 HARDNESS VALUES AT 8 DIFFIRENT SUB-LOCATIONS ON SPECIMEN 3 FROM IU3E A-146-6 (SEE TEXT)
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l 69 The EPR sensitization test was done en specimen L from location 0.25-0.75 inch. The activation peak potential for this tube was 125 mV(SCE), which indicates a very high susceptibility to IGA by poly-thionic acid. This value is not significantly different from the 110 mV
(
value obtained for other tubes.
A defect with EC indication at 3.75 inch was selected for SEM/EDAX tud metallographin examinations. A circumferential crack at 3.75 inch location was visible to the unaided eyes. Some brown color decorations around the crack also were present. Two specimens containing p
(,
the defect were prepared from location 3.5-4.5 inch, specimen El (90-180 degree) for metallographic examination, and specimen E2 (0-90 degree) for SEM/EDAX analysis.
The general appearance of the ID surface of the tube in the j '
brown cecoration area is shown in the SEM photograph in Figure 44 The surface is rough and is covered with granular and flaky deposits. Another spot from a similar area showed crusty deposits on the surff.ce, as shown in the SEM photograph in Figure 45.
EDAX analysis of the spot in Figure 45 detected only Ni, Cr, f
Fe, Ti and S on the surface. The S was present in about 0.2 weight percent concentration. Approximate concentrations of other elements on i
the spot in atom percent were: Ni-44; Cr-25; Fe-20; and Ti-0.9.
In relation to the composition of base metal, i.e., Inconel 600* rhe spot appears to be rich in Fe and Cr but depleted in Ni.
Iron in the form of oxide may have produced the brown coloration on the surface.
The apparent crack in specimen I2 was mechanically pulled apart, and the fracture surface was examined in the SEM. A SEM photograph of the fractured surface in Figure 46 shows the intergranilar nature of the crack. A photomicrograph of the same crack present in metallographic specimen El is shown in Figure 47. The crack is intergranular arid penetration is N70 percent through wall. No IGA was noticed on the ID or OD surface of the tube in the vicinity of the crack.
A transverse cross section of the tube, speci=en F 3.5-4.25 inch, 180-360 degree, showed no ICA attack on the ID or OD when exa=1:ed metallographically.
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SEM FECTOGRAYH OF A 3 ROW DECORATION ON THE ID SURFACE OF SPECDIEN E2 FROM TUBE A-146-8 1
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SDi PHOTOGRAPH OF A CRUSTY DEPOSIT IN A 3 ROW SPOT ON THE ID SURFACE OF SPECIMEN El FROM TUBE A-146-8 i
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SEM PHOTOGRAFII 0F THE FRACTURE SURFACE OF SPECIMEI E2 FROM TUBE A-146-8
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Specimen I was taken from location 6.75-7.25 inch for another SUf and EDAX examination. There was no defect indication from NDE for this location, but a shallow pit was visi51e on the ID surface. A SDf photograph of the pit is shown in Figure 48. Encrustation around the i
pit is similar to that shown in Figure 45.
EDAI analysis of the surface found, in approximate atom percent, e
elements:
Ni-44, Cr-41, Fe-12, Ti-0.8, S-0. 8, and Si and Ca in small amount 2.
Another analysis of the inside surface of the pic found the 7
deposits to be rich in Cr (76 percent) and low in Fe (~3 percent) and a
[
Ni (=17 percent). Other elements Ti, S, Ca and Si were also present in small amounts.
At one area inside the pit very high sulfur (7.8 percent) was detected, ca (0.1 percent) and Ti (2.7 percent) also were present in the area. The descaled pit is shown in Figure 49. Intergranular_ attack is clearly visible in the SDi photograph.
Specimen C, location 8.5-9.0 inch, with no apparent defect on the ID surface and no NDE indication was examined =atallographically.
IGA was observed on the ID surface of the tube,.as shown in Figure 50..
l The IGA is approximately 0.004 inch deep and 0.015 inch widc at the ID surface.
l i
A lip-crack from location 0-0.5 inch was metallographically examined. Two specimens A and C from the 0-0.5 inch location were i-prepared for the examination. Specimen A, 0-180 degree, was examined i,
in longitudinal cross sectien, whereas specimen C, 180-360 degrees, was examined in transverse cross section with respect to the tube axis.
- I Micrographs of specimens A and C are shown in Figures 51 and
$2, respectively. In specimen A, the tube wall separated at the main
' f{
crack while preparing the metallographic mount, the sepr. rated wall is visible in Figure 51. A second crack which appears to be a major branch of the main crack also is nearly through wall. The transverse section in specimen C showed three different unconnected cracks. One such crack only is shown in Figure 52; the other cracks were similar in nature.
Two specimens 3 and J from locations 8.5-9.0 inch and 10.5-11.0 inch showed no IGA attack on any surface ID or OD when examined =etal-lographically. There were no NDE defect indication at the above locations.
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MCV ' c M N0if 70:
Victor Benaroya, Chief f
Chemical Engineering Branch Division of Engineering FROM:
Conrad McCracken, Section Leader Chemical Engineering Branch Division of Engineering SUSJECT:
TNI-1 OTSG STATUS UPDATE As of November 11,1%1 kinetic expansion repairs of all tubes in both steam generators are in progress.
The first round of expansions in all tubes will be completed the week of hovember 15.
Cleanup prior to the second round of expansicos will take.pproximately 10-14 days.
The re-fora, the second round of expansions can be estimated to be finished by aid December.
We currently anticipate the licensee will submit their restart safety analysis the week of November 22, 1982.
We will distribute the safety analysis to all our consultants by express eat).
The consultant's draft TER's will be due to the staff by January 3, 1982.
The following schedule should apply for completion of our SER.
- Jan. 14 - staf f coeplete review of consultants TER, provids comments to consultants.
I
- Jan. 28 - staf f complete draf t restart SER.
- - Feb. 4 - consultants !.ubeit final TER.
l t
- - Feb. 25 - Final restart SER input pmvided to DL.
These dates will be due contingent upon the successfull demonstration
[
of serviceability for the OTSG's.
Current plans are to issue a separate d
SER to persit system heatup and leak testig of the steam generators.
Once leak testing has been cospleted, the final restert SER will be issued.
Af ter approxisetely 435 initial expansions in both steam generators were completed. 12 rew Et.T indications a re detected in tha sie-inch
[#
Qualification zone. ustnq the 8 m ; probe The majority at these n+-
indications (9 out of 151 espanded tuces in "B" and.3 out of 155 I
expanced tubes in "A") were snaii (<50* cirtuaferentiat arc ar.c a.
E h
volt or less signal)
The licensee believes that the new i ndi c a t i r-i 4
3 k
I e
s.-
V. Benaroya 2
are defects which were below the threshold of detectabili*:y prior to expansion and that expansion opened the defect wider so it became more detectable.
Based on the earlier laboratory data, it is not anticipated that the defects were caused by or propagated through wall as a con-sequence of the kinetic expansions.
Two of the 12 new indications showed larger signals; one covered
- 160* of arc and the other was a 6 volts signal.. Boroscopic examination revealed that the 160* arc signal was in fact several distinct small arc cracks that ECT was identifying as one indication.
The 6 volts signal was found to be a large shiny gouge, probably caused by a cleaning tool.
The licensee has initiated a rather extensive program to quantify the new indic-ations and assess their significance.
The significance of these new indications will be evaluated in our restart SER.
In addition to the new ECT indications, some of the tube stub sections which protrude
- 1/8" above the primerly side tubesheet and have ful)
-circumferential corrosion are being released by the kinetic expansions.
Because this is no longer a lead carrying member or leak tight joint, no significant regulatory concern exists.
The licensee wil' have to s
remove all loose parts and mill doun or otherwise smooth off all stubs which are loose to provide adequate sealing surfaces for plugs.
The cleanup and repair of this problem will be evaluated in our restart SER.
The licensee is in the process of assessing the situation and is keeping l
us informed on a daily basis. The resident inspector, with assistance L
from the TMI-2 program office, is asintaining daily cognizance of the repairs. We plan to visit the TMI-1 site with our consultants as needed to assess the repair process.
I Enclosed are copies of our consultants. C. Dodd's and D. MacDonald's trip reports from the October 18-19 meeting in Bethesda.
Conrad McCracken, Section Leader Chemical Engineering Branch Division of Engineering
Enclosure:
As stated
~
cc: w/o enclosure cc: w/ enclosure R. Vollmer POR 50-289
- 0. Eisenhut C. Cheng W. Johnston P. Wu j
l T. Novak S. Young i
G. Lainas R. Jacobs J. Knight J. Rajan l
J. Stolz L. Frank S. Pawlicki W. Seagraves, FRC T. Sullivan Dr. MacDonald, Ohio State H. Conrad R. Dillion, PNL
- 8. Liaw J. Weeks, BNL DE/CMER
DE/CMEB P. Grant C. Dodd, ORNL VBenaroya CMcCracken:a0 11/IU82 m
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