ML20132F214

Long-Term Corrosion Test Program of Nuclear Steam Generator Tubing Samples from TMI-1, Vols 1 & 2

ML20132F214
Person / Time
Site:	Three Mile Island
Issue date:	10/31/1984
From:	WESTINGHOUSE ELECTRIC COMPANY, DIV OF CBS CORP.
To:
Shared Package
ML20132F163	List: ML20132F159 ML20132F214
References
SG-85-05-008, SG-85-5-8, NUDOCS 8508020209
Download: ML20132F214 (986)

Text

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Westinghouse Electric Corporation Water Reactor Divisions St ean Generator Programs

} P.O. Box 855 Pittsburgh, PA 15230 LONG-TERM CORROSION TEST PROGRAM of NUCLEAR STEAM GENERATOR TUBING SAMPLES from THREE MILE ISLAND UNIT 1 to GPU-NUCLEAR, Reading, PA GPU-N SP-1101-22-008 FINAL REPORT Volume 1 October 1984 ,

l 8508020209 850729 PDR ADOCK 05000209 P PDR l

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L Westinghouse Water Reactor g Q855g Electric Corporation Divisions May 17, 1985 Mr. John Janiszewski GPU Nuclear Corporation i P. O. Box 1018 '

Reading, PA 19603

SUBJECT:

TRANSMITTAL 0F FINAL REPORT ON LONG TERM CORR 0SION TEST PROGRAM

Dear John:

Enclosed herewith please find 15 copies of the subject report. Additionally, we have reprinted the first and second interim reports and the Leak Rate Test Report and included them in Volume 2 for your convenience.

Should any questions arise now or in the future regarding this subject, please feel free to contact me.

Thank you for the opportunity to assist in your efforts to restart Three Mile Island Unit 1. Please contact us if we may be of further service.

Good luck in your future endeavors!

Sincerely, WESTINGHOUSE ELECTRIC C0PR0 RATION

._ec.__ k L. W. Stern SGTD - Projects Integration j /plh Enclosure cc: Mr. F. S. Giacobbe Ms. D. L. Saunders

SG-85-05-008 i

Westinghouse Electric Corporation l Water Reactor Divisions Steam Generator Programs P.O. Box 855 Pittsburgh, PA 15230

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! LONG-TERM CORROSION TEST PROGRAM i of

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. NUCLEAR STEAM GENERATOR TUBING SAMPLES i

from 1

THREE MILE ISLAND UNIT 1 a

i to i GPU-NUCLEAR, Reading, PA e

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GPU-N SP-1101-22-008 FINAL REPORT

. Volume 1 i

i October 1984 l

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TABLE OF CONTENTS I

Page

1. Introduction 1-1 1.1 The Program 1-1 1.2 Background Discussion 1-3

2. Objectives 2-1

• l 2.1 Primary Objectives 2-1 2.2 Additional Objectives 2-2

3. Program Summary 3-1

4. Facilities Description 4-1 4.1 Once-Through System 4-1 4.2 Recirculating Peroxide Loop 4-2

, 4.3 Leak Rate Measurement System 4-4 i

! 5. Specimens and Environments 5-1 l

l 5.1 Materials 5-1 5.2 Sample Configurations 5-2 l 5.2.1 Full Size Tubes 5-2 l 5.2.2 C-Rings 5-2 5.2.3 U-Bend Specimens 5-4 5.2.4 Leak Rate Test Specimen 5-4 5.3 Test Solutions

• 5-5 5.3.1 Lead Test Solutions 5-5 5.3.2 Leak Rate Test Solution 5-6 5.3.3 Ilydrogen Peroxide Solutions 5-6

6. Operating flistory 6-1 6.1 Test Parameters Recording and Control 6-1 l 6.1.1 Temperature 6-1 l

l 6.1.2 Pressure 6-1 '

6.1.3 Flow Rate 6-2

! 6.1.4 Record of Test Parameters 6-2 1

6.2 Loop Cleaning and Preconditioning 6-2 6.3 Autoclave Loading 6-3 6.4 Specimen Loads 6-3 6.5 Long Term Corrosion Experiments 6-4 6.6 Autoclave Operational Variations 6-5 6.7 Leak Rate Experiment 6-6 6.8 Chemistry Monitoring During the HFT and 6-7 First Through Fourth Operating Cycles of Lead Test 1 6.9 Chemistry Monitoring During the Fif th and Sixth 6-10 Operating Cycles of Lead Test 1 6.10 Chemistry Monitoring During the HFT, First Through 6-10 Fourth Operating Cycles of Lead Test 2 6.11 Chemistry Monitoring During the Fif th and Sixth 6-11 Operating Cycles of Lead Test 2 6.12 Hydrogen Peroxide Experiment 6-11 6.12.1 Loop Cleaning and Perconditioning 6-12 6.12.2 Loop Operation with Peroxide Additions 6-13 6.12.3 Chemistry Monitoring During the Peroxide 6-15 Expe riment 6.13 Chemistry Fbnitoring During the HFT, First and 6-16 Second Operating Cycles of Lead Test 3 and 4 6.14 Chemistry Monitoring During the Third and Fourth 6-17 Cycles of Lead Test 3 and 4

7. Results 7.1 Visual Examination 7-1 7.2 Weight Changes 7-2 7.3 Meta 11ographic Examination 7-2 7.4 Post Test Meta 11ographic Examination 7-3 7.4.1 Experimental Proceduren 7-3 7.4.2 Results 7-6 7.5 Auger and X-Ray Photoelectron Spectroscopy (XPS) 7-15 Analyses for Sulfur Pickup by New Surfaces of OTSC Tubing 11

7.5.1 Archive Tubing 7-15 7.5.2 C-Ring P2D2 7-16 1 7.6 Eddy Current Inspection Results 7-16

8. Summary and Discussion of Results 8-1 8.1 Program Summary 8-1 8.2 Discussion of Results 8-2 8.3 Ceneral Discussion 8-4

9. Appendices 9-1 9.1 Procedure for Loop Operations During Lead Test 9-2 5

i HFT Cycle 4

9.2 Procedure for Loop Operation During the Lead Test 9-4 Operations Cycles j

9.3 Methods for Preparation of Stock and Makeup Tank 9-7 Solutions

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9.4 Procedures Used During Hydrogen Peroxide Test 9-14 Operations i

9.5 Auger and X-Ray Photoelectron Spectroscopy (XPS) 9-24 i Studies of Sulfur Pick-up by Archive Tubing and Exposed C-Ring Surfaces i l  !

9.6 Eddy Current Signals from Tube Sections with Defect 9-32 Indications F

9.7 Operating Parameters for Each Autoclave, 9-68 November 1982 to May 1984 '

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I LIST OF FIGURES Pa gg, 4-1 Autoclave and Refreshed Samples Stringer with Axial 4-5 Loading 4-2 Refreshed Autoclave System Used for Once-Through 4-6 Solution Flow Through the Sample Stringer ,'

4-3 H202 Loop for CPU-N OTSG Tube Corrosion Tests 4-7 4-4 Hydrogen Peroxide Loop Syitem Consisting of Two 4-8 Autoclaves Containing Specimens Assembled for Series Flow 4-5; Schematic of Test Equipment for Leak Rate Experiment 4-9 5-1 Photographs of As-Received Material 5-8 5-2 Lead Test Specimen Bellow Loading Assembly 5-10  !

5-3 Repair Test Specimen Bellow Loading Assembly 5-11 5-4 C-Ring Specimen Configuration 5-12 5-5 Strain Cage Results 5-13  !

5-6 Zircaloy C-Ring 5-14 ,

5-7 Core Material Specimens 5-15 ,

5-8 Test Specimen Configuration for Leak Rate Experiment 5-16 j 6-1 Typical Specimen Packages; Test 3 Contains One " Lead" 6-18 Type Specimen and Cans of C-Rings and U-Bends and Test 4 Contains Two " Repair" Type Specimens 6-2 Stylized IIFT Curve 6-19 6-3 Stylized Lead Test Cycle 6-20 6-4 112 02 concentration Values 6-21 6-5 Estimated 11 022 Consumption Rates 6-22 6-6 11 022 Experiment pli Levels 6-23 i

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7-1 through Before and AFter Macrographs of C-Ring Specimens, 7-20 through !

7-23 Removed from Tests at Specified Intervals 7-42 l 7-24 through Micrographs of Exposed C-Rings Removed from 7-43 through 7-63 Tests at Specified Intervals 7-82 7-64 through Macrographs and Micrographs of C-Rings, Removed 7-83 through 7-88 Af ter Completion of Tests 7-107 7-89 through Macrographs and Micrographs of U-Bends and 7-108 through >

! 7-102 Zircaloy-4 Specimens, Removed After 7-121 i

Completion of Tests 7-103 through Post-Test Meta 11ography of Tube A16-69 7-122 through 7-107 7-126 7-108 through Post-Test Meta 11ography of Tube A88-7 7-127 through ,

7-112 7-131 j

7-113 through Post-Test Meta 11ography of Tube A13-63 7-132 through 7-124 7-143 t

7-125 through Post-Test Meta 11cgraphy of Tube A24-94 7-144 through 7-143 7-162 7-144 Leak Rate vs Axial Load for the Seven Test Runs 7-163 7-145 through Meta 11ography for the Leak Rate Test Piece 7-164 through 7-171 7-186 9-1 Titration Curve i 9-20

9-2 Normalized Sulfur Peak-to-Peak lleight vs 9-26 Depth Below the Surface for Three tou- "

Implanted Standards '

l 9-3 Calibration Curve for Sulfur Analysis in Inconal 9-29 l Alloy 600 by AES 9-4 through l

Eddy Current Signals from Long Term Corrosion 9-33 through 9-38 Test Tube Specimens 9-67 l

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2 LIST OF TABLES l

5-1 TMI-1 Full Size Tube Identification 5-17 5-2 Inconel 600 C-Ring Material Identification 5-18 5-3 Composition of Alloys Used to Prepare Mint-U-Bends 5-20 5-4 Alloy Supplier, llent No., and Form 5-21 5-5 Alloy lleat Treatment and Mechanical Properties 5-22 5-6 Alloys and U-Bend Coding 5-23 5-7 Long Term Corrosion Test Chemistry Specification 5-24 5-8 Chemical Composition of Makeup Tank Solutions 5-25 (Leak Rate Measurements) 6-1 Autoclave Specimen Loading 6-24 6-2 C-Ring Replacement Sequence 6-26 6-3 Analytical Data for Test 1 - IIFT Cycle 6-28 6-4 Analytical Data for Test 1 - 1st Operating Cycle 6-29 6-5 Analytical Data for Test 1 - 2nd Operating Cycle 6-30 6-6 Analytical Data for Test 1 - 3rd Operating Cycic 6-31 6-7 Analytical Data for Test 1 - 4th Operating cycle 6-32 6-8 Analytical Data for Test 1 - 5th Operating Cycle 6-33 6-9 Analytical Data for Test 1 - 6th Orarating Cycle 6-34 6-10 Analytical Data for Test 2 - IIFT Cycle 6-35 6-11 Analytical Data for Test 2 - 1st Operating Cycic 6-36 6-12 Analytical Data for Test 2 - 2nd operating Cycic 6-37 6-13 Analytical Data for Test 2 - 3rd Operating Cycle 6-38 6-14 Analytical Data for Test 2 - 4th operating cycle 6-39 6-15 Analytical Data for Test 2 - 5th Operating Cycle 6-40 6-16 Analytical Data for Test 2 - 6th Operating Cycle 6-41 6-17 Analytical Chemistry Results for Loop 3 During Cleanup 6-42 and Preconditioning vi l

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i 6-18 Analytical Chemistry Results for Loop 4 During Cleanup 6-43 l

and Preconditioning 6-19 Apparatus Changes and Events: Peroxide Cleaning Runs 6-44 6-20 Average Daily Makeup Tank Peroxide Concentrations 6-45 and pH Values  :

6-21 Daily Peroxide Usage 6-46 1 6-22 Peroxide Loop Analytical Data 6-47 l

6-23 Analytical Data for Test 3 - IIFT Cycle 6-50 6-24 Analytical Data for Test 3 - 1st Operating Cycle 6-51 i j 6-25 Analytical Data for Test 3 - 2nd Operating Cycle 6-52 j 6-26 Analytical Data for Test 4 - IIFT Cycle 6-53 '

6-27 Analytical Data for Test 4 - 1st operating Cycle 6-54 6-28 Analytical Data for Test 4 - 2nd Operating Cycle 6-55 i 6-29 Analytical Data for Test 3 - 3rd operating cycle 6-56 6-30 Analytical Data for Test 3 - 4th operating Cycle 6-57 6-31 Analytical Data for Test 4 - 3rd Operating Cycic 6-58

{ 6-32 Analytical Data for Test 4 - 4th operating Cycle 6-59 L

l 7-1 TM1 C-Ring Weight Heasurements 7-187  !

j 7-2 fummary of C-Ring Evaluations t 7-189 }

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j 7-3 Summary of Full Tube Specimen Defects 7-191 1 l i

7-4 Summary of Tube Eddy Current Inspections 7-135

) 7-5 Average Leak Rate Measurements of THI Tubing 7-199 l 8-1 Exposure Summary 8-12 9-1 Fraction of Sulfur Atoms Stopped Within a 10 NM Slice 9-27 of Material at Various Depths Below the Surface i

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1. INTRODUCTION  ;

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1.1 The Program i

j The GPU Nuclear Corporation (GPU-N) is engaged in a repair j program for the nuclear steam generators at its Three Mi.to Island Unit 1 (TMI-1) generating plant. A part of that program include:s the establish-l' ment of the long-term corrosion behavior of steam generator tubo samples. [

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from the TMI-1 steam generators, under a programmed exposure of both repre- l sentative and nonrepresentative reactor coolant chemistry, plus representa-I tive temperature and load variations. This long term corrosion test (LTCT) program is being conducted for CPU-N by the Westinghouse Electric Corporation through the Westinghouse Steam Generator Programs Activity which sponsors the testing operations at the Westinghouse Corporate R and D Center. '

f The purpose of this program, as stated in the GPU-N Short Form l.

Specification SP1101-22-008 Revision 2 (Reference 1), is to demonstrate that the processes of kinetic expansion, and sulfur oxidation during peroxide  ;

cleaning and plant operation will not result in propagation of existing ICSAC, '

] initiation of new ICSAC, or other corrosive damage using the proposed new THI-1

! chemistry control specifications.

l The CPU-N Specification (Reference 1) was transmitted to Westinghouse under a cover letter of July 13, 1982, by F. S. Giacobbe, i

Manager, Materials Engineering and Failure Analysis, GPU-N. That cover  !

1etter requested that the contractor's program include two interim reports l and a final report. The present report is the final report and as such is '

a combination of the first and second interim reports which are structured l into the Westinghouse agreements with CPU. This report covers all program 7 l activities from inception date to completion of the program in September 1984 i

as delineated in Section 3. Program Summary. The new material presented I horoin encompasses the fif th and sixth cycles of Icad testa 1 and 2 I

! the third and fourth cycles of lead tests 3 and 4, and the results of all metallographic examinations of the sampics investigated. -

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This final reporting effort is divided into 2 volumes. Volume 1 contains the Final Report as a summary of the first (November 1982 to April 1983) and second interin reports (May to December 1983) along .

with newly acquired data since January 1984. Volume 2 contains unabbreviated copies of the first and the second( ) interim reports along with a full copy of the " Leak Rate Report" (Document 83-5D2-TMISG-RI) .

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1.2 Background Discussion The two nucicar steam uenerators of the TMI-l facility are the once-through steam generator (OTSC) design furnished by the Babcock and Wilcox Company. As part of that supplier's manufacturing sequence, the entire finished OTSG is given a stress relief heat t reat men t , the time and temperature cycle of which creates a grain boundary chromium depleted (CBCD) microstructure in the nickel-chromium-iron alloy (inconel Alloy 600) which in the tubing material of the generator.

Extensive testing of this microstructure in aqueous environments which can cause elevated temperature caustic stress corrosion cracking (SCC) has demonstrated that the CBCD condition is as least as resistant as, if not more resistant than, the " mill annealed" condition to the typically intergranular caustic SCC form of degradation (References 5-10). Other tests have demonstrated that the CBCD microstructure possesses high resistance to the "Coriou" type of phenomenon, an intergranular cracking process requiring high stress, or high strain, or a high strain gradient, coupled with a typically prolonged exposure at elevated temperatures () 6000 F) to high purity water (Reference '51).

The only extensively investigated conditions which demonstrate that the CBCD condition is selectively susceptible to intergranular forms of degradation are at los temperatures (at or near room temper-ature, for example) in aqueous species which are not representative of normal nuclear steam generator environments. Apart from boiling nitric acid solutions (the "Huey" and " modified llucy" tests), there exist certain sulfur-containing oxyanions which can be deleterious in low temperature aqueous anlutions to iron chromium-nickel alloys in general, if these alloys possess the CBCD structurn. In these potentially aggressive oxyantons, the oxidation state of sulfur is less than 6+

(or VI), onecios such as tetrathinnate ($46 0 ) thiosulf ate (5 0$"), or 2

"polythlonic acid (H2Xy8 0 ) having received attention in recent years (References 12 and 13. This form of intergranular attack (which is selective to and requires the GBCD structure) has not been identified fortheverycommonsulfateion,50{',however. Definitive identified 1-3

1 observations of the relatively high resistance of the GBCD structure, compared to the " mill annealed" condition, to intergranular attack in acid sulf ate solutions hsvo recently been published under EPRI sponsorship. These tests, which used 80,000 ppm Na2504 at an initial room temperature pH of 3 (obtained with H SO 2 4), showed that the GBCD condition was at least as resistant as the " mill annealed" condition of the same he.it, in 5000 hour0.0579 days <br />1.389 hours <br />0.00827 weeks <br />0.0019 months <br /> exposures at 6300F (Reference 14).

4 The low-temperature reduced sulfur oxyanion attack of GBCD Inconel 600 renains one of the few cases to which the GBCD condition can be demonstrated to be selectively sensitive. A detailed, failure an,slysis of TMI-1 OTSC tubing which exhibited primary-side-initiated intergranular attack and intergranular cracking has led GPU-N to conclude that low-temperature sulfur-species attack was responsible (Reference 15), This conclusion is also supported by additional failure analysis reports (References 16, 17, 18, 19). Both References 15 and 16 provide possible sources of an ingress of sulfur species into the reactor coolant system during the prolonged layup of TML-1, and both documents address mechanistically plausible chemical scenarios for the production of an nearessive aqueous low-temperature sulfur-bearing species. It is the TM1-1 OTSG tubing which has had the history outlined above and detatted in Ref erence 15 which is the subject of the current j

LTCT program.

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I j 2. OBJECTIVES 2.1 Primary Objectives The two initial objectives of the LTCT program are responsive to the GPU-N Specification and were (1) the determination of the long-term corrosion and stress corrosion performance of service-exposed TMI-1 OTSG tubing material from the generators and (2) the identification of any potential in plant corrosion issues and the conditions for such issues. The tests are to be performed using reactor coolant chemistry composition representing the upper bound of specified limits for contaminants. The GPU-N Specification provides the chemistry limits and time and temperature cycles for the tests.

To meet program objectives,four types of specimens were utill ed in four separate test vessels. Specimens consisted of full section.

l axially loaded " Lead Test" and " Repair Test" specimens. C-ring, and i

U-bend specimens. " Lead Test" and " Repair Test" specimens were prepared l f rom service exposed Unit 1 steam generator tubing which had been removed from the upper tubesheet region. " Lead Test" specimens I consisted of open lengths of tubing while " Repair Tests" specimens consisted of tube /tubesheet mockups prepared by explosively expanding tube sections into an outer collar following a procedure which duplicates repairs performed on Unit 1. C-rings, which were loaded to place I.D. surfaces in tension, were prepared from both service exposed and archive (non-service exposed) tubing. U-bends were prepared from other materials used in the fabrication of Unit I core structural components.

The test operational sequences used fnr each test simulated conditions encountered in plant operationn and were, with minor variations,  ;

identical in all tests. The major difference hotween tant' environments 2-1

was that one contained thiosulfate and the remaining three contained sulfate additions.

2.2 Additional Objectives Additional secondary objectives, not originally included in GPU-N Specification have been identified and met as the LTCr program l

and on-site operations at TMI-1 have proceeded. The chief of these secondary objectives became the development of equipment for and the achievement of the hydrogen peroxide cleanup of selected OTSG samples for the subsequent inclusion of such cleaned samples into the LTCT.

Another secondary objective which is an outgrowth of the preceding cleanup activity became and is the verification of the performance of stressed alloys representative of in-core materials when such materials are (1) pre-exposed to a " conditioning" of reactor coolant (containing approximately 100 ppb of 504 ), (2) exposed to the I

hydrogen peroxide cleanup cycle, and (3) subsequently exposed for prolonged periods to the " worst case", but normal, reactor coolant chemistry programmed by (and identical to) the main LTCr program.

A third secondary objective was to determine, using Auger electron spectroscopy (AES), how much sulfur (in ug/cm2) is present within the first 100 nm of the inside (10) surfaces of GPU-N steam generator tubes that were conditioned to simulated reactor coolant chemistry at elevated temperatures af ter peroxide cleaning, using standards prepared by ion implantation to calibrate the AES technique, and X-ray photoelectron spectroscopy (XPS) to identify the sulfur compoundt, present.

As a fourth secondary objective--a leak rate experiment was performed on a CPU supplied section of TMI Unit #1 steam generator tubing. The specimen contained a small circumferential through-wall crack detected by eddy current analysis. The purpose of the experiment was to determine I

the primary to secondary leak rate at operating temperatures and tube pressure dif ferentials under a range, of axini load conditions. At the f

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conclusion of.the leak rate experiment, an extensive microscopic and electron optical examination was performed to aid in determining an effective cross-sectional area of the defect.

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l 3. PROGRAM SL7 DIARY l

The program plan has undergone several iterations, modifications

! and alterations of scope since its inception under the original GPU-N Specificatiorb) As finally structured, the program consists of four principal elements.

1. Two extended duration " Lead Tests" (Loops 1 and 2) using

" Lead Test Samples", as defined in Reference 1.

These tests started in October, 1982 and continued through June, 1984

2. A hydrogen peroxide cleanup run to simulate the treatment of the TMI-1 primary system. This test applied to one " Lead Test Sample" (Loop 3), two " Repair Test Samples" (Loop 4),

and " Core Material Samples" as defined in Reference 1 and this report. It was completed in March, 1983.

3. Two additional " Lead Test Type" extended-duration corrosion tests using the " Repair, Lead, and Core Material Samples" of Item 2 above after they completed the peroxide cleaning phase.

These tests started in May 1983 and were continued through May, 1984 using the same " Lead Test" operational sequence as the Item 1 tests. These test loops were subjected to a HFT cycle and only four operational cycles as opposed to the six operational cycles of Loops 1 and 2.

4. A leak-rate experiment to subject a defective section of

'INI-1 steam generator tubing to operating temperature and j primary to secondary pressure differential conditions in water. (The defect was identified as a circumferential, l

fully intergranular crack.) Leak rates were measured as a function of axial load on the tube.

The first interim report (Volume 2.1) encompassed Item 1. Lead Tests 1 and 2, for their ilFT, first and second cycle, and the entirety of item 2, the peroxide clean-up, and as such, delineates the test matrix (of samples) which constitutes Item 3, the Icad test type program with the peroxide-cleaned samples.

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Item 1, the two long-term " Lead Tests", followed essentially the plan originally given in Reference 1 and has consisted of two tests which differ only in the make-up sulfur-dosing species to the otherwise normal reactor coolant simulated chemistry (Li, B, H2 , etc.) .

Test i used thiosulfate and Test 2 used sulfate. Both sulfur anions are at specified levels (100 ppb, nominally). Both tests follow the same operational sequences which are:

(1) Hot Functional Test (HFT) Stage (2) Cycle 1 (3) Cycle 2 (4) Cycle 3 (5) Cycles 4-6 The cycles differ in the amount of B, as H3B03 , and Il as LiOH, which are present in the test solutions and which are varied to simulate plant operations.

The second interim report (Volume 2.2) covered the two lead tests.

Item 1, from the start of the third cycle through cycle 4, also the two additional " Lead Test Type" extended-duration corrosion tests for the HFT and Cycles 1 and 2 (Item 3). As noted, the report also covered the highlights of the " Leak-Rate-Report" (Volume 2.3) which constitutes Item 4.

The present final report is a combination of the first and second interim reports (November 1982 to Sept. 1984). Also included are the two lead tests, Item 1, from the start of the fifth cycle through the sixth cycle,and Item 3, the two extended duration corrosion tests with the pe,,roxide cleaned samples for their third and fourth cycles. These data have been acquired since Jan. 1984 and represent the conclusion of the corrosion testing.

A very detailed effort in this report has been devoted to the in-depth metallographic examination of the exposed samples in combination with eddy current investigations.

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4. FACILITIES DESCRIPTION 4.1 Once-through System The once-through system shown schematically in Figure 4-1 and in i

the photograph of Figure 4-2 is the basic apparatus used for all long term corrosion testing of GPU-N OTSG Inconel tubing. The basic element of this apparatus is a standard Autoclave Engineers 2-liter, bolted closure autoclave, which contains the test specimens. These specimens, which are samples of axially loaded GPU-N OTSG Inconel 600 tubing, and cans of C-ring or U-bend samples (depending on the individual test specifications), are plumbed for a series flow of solution upward through the samples. Entry ports (feed-throughs) in the autoclave head provide the means of nitrogen gas pressurization of the bellows of the specimen loading fixture as well as entry and egress of the tubing which s carries the test solution to and from the specimens.

The first item in succession of the flow-through apparatus is a stainless steel makeup tank (MUT) with a nominal 70 1 capacity, which is filled with 50 1 of the test solution. The MUT is equipped with a sight tube to monitor the liquid level of the test solutions, and ports to provide means of solution exit, sparging, and pressurizing (gas over-pressure). The second item in series, following the MUT is a Whitey Model LP10 feed pump which is adjusted to maintain a 100 al/h (ideal) '

flow of the test solution through the system. The test solution flows through a check valve, into the autoclave, internally through the l

specimens, and exits the autoclave through a cooler composed of coiled stainless steel tubing. The cooler effluent discharges through a Controlmatic back pressure (BP) regulator, which provides the method of regulating the solution pressure. Located down-stream from the BP regulator is a tap for effluent sampling and, piped in parallel, a flow 4-1

i meter (F/M) to measure system flow rate. Finally, the effluent is collected, monitored and disposed of in accordance to Nuclear Regulatory Commission requirements.

Ports on the autoclave body are used for filling, evacuation, sparging and for the attachment of the rupture disk (R/D) and BP regulator necessary for controlling the autoclave pressure. Both the autoclave rupture disk and the BP regulator are plumbed to the radiation monitored collection drum for safety in event of an overpressure release.

The autoclave is heated by means of external clamp on resistance heaters. Normal safety and control equipment are used with each autoclave system.

This basic system has been used to conduct both the HFT and Lead Test Operations for all four tests. The detailed operating procedures for HFT and operations cycles are presented in Appendix 9.1 and 9.2, respectively, a

4.2 Recirculating Peroxide Loop Plans called for exposing the primary system of TMI-l to a i

hydrogen peroxide solution to ensure that any residual sulfur species will be oxidized to the sulfate form prior to system heat up. GPU-N elected to have the test specimens for Tests 3 and 4 of the existing program also exposed to this peroxide clean up operation.

In order to accomplish this, the once-through systems of Tests 3 and 4 were modified to produce a series recirculating system.

Additional changes to the loop system during the peroxide cleaning cycle were made to improve operating efficiency or to meet contingencies. The ,

peroxide loop cleaning system, in its final form, is delineated in Figure 4-3, and shown photographically in Figure 4-4.

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In essence, the H 022 lo P consisted of two once-through systems in a series loop fed by a single make-up tank. As previously described for the once-through system, the flow of the H 02 2 cleaning solution through the GPU test specimens within the autoclaves was in a series configuration.

The circuit flow f rom the MUT, through the autoclave and back to l

the MUT is straight-forward. The test solution is pumped from the MUT by a circulation pump at the rate of ~ 7 1/h. A rupture disk, plumbed to return the test solution to the MUT in the event of over pressuri-zation of the system is located downstream from the pump. It is followed by a stainless steel surge bottle half filled with inert gas.

the function of which is to dampen pressure fluctuations resulting from pump operations. The test solution, which is pre-heated by flowing through a regenerative heat exchanger and heating tape covered tubing prior to entering the first autoclave, flows serially through the GPU-N specimens and exits the autoclave. The solution flow through the second autoclave and GPU-N specimens is similar to that of the first auto-clave. After leaving the second autoclave, the hot test solution again etters the regenerative heat exchanger, with the purpose of heating the l

l solution about to enter the first autoclave. Following the regenerative I

' heat exchanger in the loop in the order stated are a cooler, a BP regulator to control the test solution pressure, a flow meter, a 4-way valve, a chemical addition system, and the MUT. The normal solution flow direction is upward through the stainless steel chemical addition pressure vessel to assure complete addition of the chemicals.

It is appropriate to note the valving arrangements at the autoclaves which permitted preconditioning of the loop tubing with the autoclaves and samples isolated. Also noteworthy is the tubing from Autoclave 2 to the MUT return line, necessitated by the leakage of a Repair Test sample tube weld. This circuit returned to the MUT the very small volume of solution passing through the weld defect and, thereby, l

maintained the AP across the tube constant.

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One of the first revisions to the apparatus was the addition of an automatic chemical injector which allowed continuous addition of hydrogen peroxide to the loop and eliminated the need for discrete hourly manual H 02 2 additions. It was also necessary to add a recirculation pump to assure rapid mixing of all chemical additions to the system.

4 Other valving and port arrangements in the chemical addition and loop system permitted pressurization, evacuation, and chemical pressure vessel drainage when necessary.

The final system was a product of continuous refinement and improvement throughout the 500 hour0.00579 days <br />0.139 hours <br />8.267196e-4 weeks <br />1.9025e-4 months <br /> peroxide cleaning (exposure) operation.

4.3 Leak Rate Measurement System The test autoclave equipment was based on that being used for the long-term corrosion tests.(2) The original test stand was modified by installing an autoclave effluent line through a cooling coil and back pressure regulator. A simplified schematic diagram of the test system is shown in Figure 4-5.

W 4-4

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-  :: 2 P

Sparge MUT h System

-100 cc/hr 50 1 Aut lave Pump ][ sg 2: v v

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C-Rings p/g y

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JI N Sparge  ::  ::ECT Caps 2 V CV Monitor Drain Figure 4-1. Autoclave and Ref reshed Sample Stringer with Axial Loading.

4-5

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4-6

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Figure 4-3. H022 Loop f or GPU-N OTSC Tube Corrosion Tests.

4-7

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. Tank E Cooling Backpressure a Colls Regulators

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& o Leakage Through

= 9 Specimen Defect

-+ Pump Figure 4-5. Schematic of Test Equipment for Leak Rate Experiment.

5. SPECIMENS AND ENVIRONMENTS 5.1 Materials j Test materials included Inconel 600 steam generator tubing and various reactor core materials. The steam generator tubing was supplied by GPU-N either as sections removed from TMI-1 or as archive OTSG tubing. Tubes from TMI-1 were supplied both with and without eddy current detected defects. The defects were ID-initiated, circum-ferential cracks, some of which were through-wall. Tubes for full size specimen testing were received with end pieces welded on. The archive 1

tubing previously had been mill annealed plus stress relieved at 1150 0F for 18 hrs.

Photographs of the as-received tubes are shown in Figure 5-1.

The identifications of the full size tubes are given in Table 5-1.

Table 5-2 presents the identification of material used to make C-rings.

The compositions of the reactor core materials used to prepare mini-U-bends are given in Table 5-3. The only material that could not be traced to a heat number and composition was wire which was labeled 308L. An analysis made on the scanning electron microscope with the energy dispersive X-ray spectrometer (EDS) was consistent with the wire being 308L. In Table 5-4 are given the alloy supplier,' heat number or heat treatment code, and alloy form. The heat treatments used and the mechanical properties are tabulated in Table 5-5 and' the coding of the specimens in Table 5-6.

All heat treatments by Westinghouse were in dry hydrogen.

l 5-1

l 5.2 Sample Configurations Specimens were configured as stressed, full section tubes, C-rings and U-bends. The full section tubes were supplied by GPU-N in either a " lead" or

" repair" test configuration.

5.2.1 Full Section Tubes l In the present LTCT, the " Lead" specimens correspond to the free standing tubes in the steam generator while the repair tests simulate explosively expanded tubing within and just below the tubesheet. Five o f the specimens were lead type, while B94-27(4 1/2 to 101/2) and A24-94(36-42) were repair specimens.

Both types of specimens were tested under a 500 pound load except during temperature cooldowns to ambient when the load was increased to 1100 lbs. These loads are representative of those which would exist on OTSG tubes during operation and normal cooldowns, respectively. Loads were obtained with a bellows actuated rig which allowed remote adjustment at any time.

Photographs of the bellows assemblies for each specimen type are shown in Figures 5-2 and 5-3. By pressurizing the bellows, an axial tensile load can be placed on the tube. Each bellows assembly was j

l calibrated prior to use by pressurizing to 3000 psi and measuring the l

l resulting specimen deficction. Specimen load was then calculated t

from the elastic modulus and dimensions of the tube.

5.2.2 C-Rings-Inconel C-rings were made from 3/4" lengths of tubing per the schedule shown in Table 5-2.

After transversely cutting, each specimen was drilled to take a loading stud and then slotted. The loading method is illustrated in Figure 5-4. An Inconel 600 stud protruded f rom a hole in the tube at 90 to the desired stress location. The stud was held in place with a nut inside the tube and a locating depression diametrically opposite the stud hole. The C-ring was loaded by turning the stud while holding the nut stationary.

5-2

, , ,,, n- ,- - - , . -

s After loading the C-ring, a second Inconel 600 nut was used to lock the stud into place.

Three archive and fcur service tube C-ring specimens were strain gaged to determine the relationship between specimen strain and opening displacement.

Initially, a biaxial gage was applied to an archive specimen with the following results:

i Deflection *circumferential " axial (mils) (u strain) ( strain) 0 0 0 286 8 3.3 573 10 1146 8 10.0 1718 4 2291 6 16.6 2864 4 ,

This test indicated that the axial strain component was insignificant. Only uniaxial gages in the circumferential direction were applied to the remaining specimens.

An LVDT-based diameter measuring device was developed and calibrated for determining specimen displacement. Using this device the strain vs. displacement curves shown in Figure 5-5 were determined.

Displacement was limited to 7 mils to avoid gross plastic deformation of the specimens. Subsequent tests verified that the strain vs.

displacement relationship remained linear to at least twice this displacement value.

Based on the minimal scatter shown in the strain gage data, all specimens were loaded to a displacement of 13.7 mils prior to autoclave exposure. This value was extrapolated from Figure 5-5 to meet the request of GPU-N to strain the C-rings to 0.25 percent (2500 p strain). )

1 5-3

All C-rings were weighed to the nearest 10 pg and macrophoto-graphs of the stressed ID area were taken.

The test configuration for the OD loaded Zircaloy 4 C-ring is shown in Figure 5-6. The specimen deflection used was 0.08 inches which is about 25 percent above the yield strain of the material. Type 304 stainless steel bolts and' nuts were used to load the Zircaloy 4 C-rings.

5.2.3 U-Bend Specimens Various reactor core materials were included in the experiment as miniature U-bend specimens.

The blanks for mini-U-bends were approximately 1.5" x 0.25" x 0.030". For specimens with welds, the filler metal was deposited by the TIG process at a location corresponding to the eventual apex and element of the U-bend. A U-bend was made by bending the blank around a 1/8-in.

diameter mandrel and bolting the legs parallel with an austenitic stainless steel nut and bolt.

Figure 5-7 is a photograph of all of the U-bend specimens.

5.2.4 Leak Rate Test Specimen The test specimen (0.625 in. OD, 0.037 in. wall) was welded into a bellows loading rig (Figure 5-8) developed for long range corrosion testing of similar TMI tubing. The loading rig was modified by the addition of a set of turnbuckles to allow compressive loading of the specimen so that a net zero load condition could be achieved at the desired test pressure differential.

Zero load conditions were established using outputs f rom three strain gages placed at 120' increments around the circumference of the test i

5-4

l sample. As the sample was pressurized to the expected test AP of 1175

.l psi, the turnbuckles were tightened to maintain a balanced zero axial load. When the pressure was released, the turnbuckles maintained a ,

small compressive load on the tube which would return to zero when the i

approximately 1175 psi pressure differential was established during the leak rate test. Additienal axial loadings were achieved by pressurizing j a bellows which was linked to the ends of the specimen. *

5.3 Test Solutions 5.3.1 Lead Test Solutions 1

i Tne preparation of the Lead Test solutions followed a systemized procedure which is briefly summariced here. A comprehensive description 1

of the Lead Test Solution preparation is given in the Appendix 9-3.

Stock solutions were prepared from the reagent grade salts of

} lithium hydroxide sonohydrate (LiOH+H 2 O), sodium fluoride (NaF), sodium chloride (Nacl) sodium thiosulfate pentahydrate (Na2 S0 2 3 5H 2O) and sodium sulfate decahydrate (Na2 SO4 +10H2 O). i The nominal concentrations of the stock solutions were 5000 ppa

~

Li+, 1000 ppa F , 1000 ppa C1~, 1000 ppe S 23 0 , and 1000 ppa SO 4-i j In preparing an individual Lead Test solution, a weighed amount

) of United States Borax and Chemical Company Special Quality boric acid was dissolved in deionized water in a polyethylene holding tank.

Aliquot volumes of the Li, and SO4 (or S23 0 , depending on the test solution) stock solutions were added and the solution in the holding tank was deaerated by sparging with nitrogen. Prior to transfer of the test solation from the holding tank to the MUT, and just prior to the test startup, a weighed amount of 65 percent aqueous solution of hyder.zine and agraliquot volumes of F' and Cl were added to an in-line addition vessel. During the transfer process, these species are mixed i

t 4

5-5

_ _ _ _ _ __ _ , _ ~ _ - _ .., . _ _ . _ _ _ _ . _

with solution from the holding tank and flushed into the MUT. This procedure was used to minimize the loss of hydrazine and to avoid ,

~

adsorption of F- and C1 on the walls of the polyethylene holding tank.

The nominal chemical compositions for the individual Lead Test solutions are given in Table 5-7. The sulfur species for " Solution 1"

] (GPU-N designation) is exclusively thiosulfate as shown in Table 5-7; for " Solution 2" it is exclusively sulfate.

S.3.2 Leak Rate Test Solution The composition of the test solution is shown in Table 5-8. )

I It represents an actual analysis of the solution used in this test. It was made up from the same stock solution (Solution 2) prepared for the lead tests as described above.

4l

(

5.3.3 Hydregen Peroxide (H 220 ) S luti ns i

The 500 hour0.00579 days <br />0.139 hours <br />8.267196e-4 weeks <br />1.9025e-4 months <br /> pre-operational exposure of the GPU-N specimens to ,

hydrogen peroxide solution was performed in a recirculating loop system according to the detailed operating procedure delineated in Appendix 9-4.

The initial composition of the 501 of solution in the MUT con-sisted of 2350 1 50 ppm boron (as H 3 B0 3 ), 1.2 to 2.2 ppm lithium (as LiOH) and 0.100 1 0.05 ppm sulfate (as Na 2SO 4 ). The lithium and sulfate (SO 4

) were added as aliquots of the stock solutions described in Section 5.3.1. The pH of this solution was adjusted to 8.0-8.2 with

! concentrated (28-30 percent NH 3) amm nium hydroxide (NH40H).

Hydrogen peroxide (H 22 0 ) initially was added manually to the loop in hourly increments. Subsequently an automatic, chemical addition system was used to make periodic additions of a 50,000 ppm H 022 stock solution.

The peroxide stock solution was prepared by weighing 166.7 g of Perone 30 EG hydrogen peroxide (30 percent H 022 by weight) into a 1 liter volu-4 metric flask and diluting to volume with water. All of the water used for E. I. DuPont de Nemours, Inc. , Industrial Chemical Division, Wilmington, DE.

5-6

i soluci:n preparation and dilution was high purity deaerated deionized water, with a conductivity of approximately 0.1 umho.

Other precedures required for test operation during the peroxide exposure are also found in Appendix 9-4.

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Figure 5-3. Repair Test Specimen Bellow Loading Assembly 6

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

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TMI C RINGS 1500 l A = 1E7 1400 -

B = 1E8 C = 1 A6  !

e 1300 -

D = 104 E = 286 , /@

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DISPLACEMENT (MILS)

Figure 5-5. Strain Gage Results

. 5-13 w

i e.375 --->

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L/2 L/2

• -- 0.331 -> * .022 e- -* e- -*

I . _ _ _ ._____

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Ri\)!' NO. 4 40 We TYPICAL TYPICAL 80s IDENTIFICATION NUMBER 1

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I Figure 5-8. Test Specimen Configuration for Leak Rate Experiment i ,

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I 5-16

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i i i Table 5-1 TMI-1 FULL SIZE TUBE IDENTIFICATION Defect Specimen Test Tube Section(l) Heat No. Location (I) Type Loop A24-94 19-5/16" 7/16" M2409 None Lead 1 A13-63 11" 9/16"* M2408 16" Lead 1 B16-22 52" - 59" M2800 None Lead 2 A88-7 2" 3/4" M2560 6" Lead 2 A16-69 6-1/2" 1/4" M2345 9" Lead 3

) A24-94 36" - 42" M2409 None Repair 4 B94-27 4-1/2" 1/2" M2869 None Repair 4 I

1 (1) Dimensions from original top of tube in the OTSG.

• Specimen reduced in size before start of test I

>i l

1 4

5-17

. .~ . -- .

Table- :i-2 INCONEL' 600 C-RING MATERIAL IDENTIFICATION 1 ' C-ring Slot (2)

Number Tube Location (I) Angle Heat 1A1 A 88-7 9-3/4" 1/4" 180 M2560 1A2 A 88-7 9-3/4" 1/4" 270 0 M2560 0

l 1A3 A 88-7 9-3/4" 1/4" 0 M2560 0

d 1A4 B111-62 237-5/8" - 240-5/8" 90 M2560

1A5 B111-62 237.-5/8" - 240-5/8" 180 M2560 1A6 B111-62 237-5/8" - 240-5/8" 90 M2560 151 A 24-94 25-7/16"- 30-13/16" 180 0 M2409 152 A 24-94 25-7/16"- 30-13/16" 270 M2409 153 A 24-94 25-7/16"- 30-13/16" 00 M2409

) IB4 A 24-94 25-7/16"- 30-13/16" 90 M2409 185 -

A 24-94 25-7/16"- 30-13/16" 180 M2409 1D1 B 94-27 18-1/2" 1/4" 180 M2869 1D2 B 94-27 18-1/2" 1/4" 270* M2869 i

1D3 B 94-27 18-1/2" 1/4" 0* M2869 i

1D4 B 94-27 18-1/2" 1/4" 0' M2869 2A1 A 13-63 20-9/16"- 23-9/16" 180 M2408 i 2A2 A 13-63 20-9/16"- 23-9/16" 270 0 M2408 0 M2408 2A4 A 13-63 38-1/8" 1/8" 0 2A5 A 13-63 38-1/8" 1/8" 90 M2408 0

2B1 B 16-22 59" - 64" 180 M2800 ,

2B2 B 16-22 59" - 64" 270 M2800 2B3 B 16-22 59" - 64" 0" M2800 0 M2800

! 2B4 8 16-22 59" - 64" 90 2B5- B 16-22 59" - 64" 180 M2800 B 16-22 59" - 64" O M2800 2B6 0

ID5 B 34-19 10-1/2" 1/2" 180 M2869 B 34-19 10-1/2" 1/2" 270 M2869 l ID6 1D7 B 34-19 10-1/2" 1/2" 0" M2869 8 34-19 10-1/2" 1/2" 180 M2869 j

ID8 1D9 B 34-19 10-1/2" 1/2" 180' M2869 (1) Dimensions from original top of tube in the OTSG.

j (2) Location of C-ring cutout, per GPU-N ref erence angles.

Looking down tube, the angle increases clockwise with 0 at 6 o' clock 90 at 9 o' clock,180 at 12 o' clock, etc. The slot . (cutout) occurs 1800 from the resultant maximum stress on the C-ring.

5-18

[

l y, . .. _ . , , _ . . , . . _ . . - _ _ , _ . . _ _ . _ - _ _ . . . _ . , _ _ - , _ .,

Table 5-2 (Continued)

C-ring Slot (2)

Number Tube Location II) Angle -

Heat 2D1 A 16-69 2" 6-1/2" 180 M2345 2D2 A 16-69 2" 6-1/2" 270 'M2345 2D3 A 16-69 2" 6-1/2" O M2345 1El Archive Material M2320 1E2 Archive Material M2320 1E3 Archive Material M2320 1E4 Archive Material M2320 1ES Archive Material M2320 1E6 Archive Material M2320 1E7 Archive Material M2320 PIA 1( ) A62-8 5" - 11" 0* M2560 PIA 3 A62-8 5" - 11" 90* M2560 PIA 4 A62-8 5" - 11" 180 M2560 PIA 4 A62-8 5" - 11" 270" M2560 PIAS A62-8 5" - 11" 00 M2560 P2D1 A12-62 2" 4-1/2" 0 0 M2345 P2D2 A12-62 2" 4-1/2" 90* M2345 P2Al A37-29 49-1/2" 1/2" 0 0 M2408 P2A2 A37-29 49-1/2" 1/2" 900 M2408 P2A3 A37-29 49-1/2" 1/2" 180 M2408 l P2A4 A37-29 49-1/2" 1/2" 270 M2408 P2A5 A37-29 49-1/2" 1/2" a0 M2408 P1D1 B34-19 6-1/2" 1/2" 0 M2869 P1D2 B34-19 6-1/2" 1/2" 90 M2869 P1D3 B34-19 6-1/2" 1/2" 180 M2869 P1D4 B34-19

6-1/2" 1/2" 270* M2869 P1D5 B34-19 6-1/2" 1/2" 00 M2869 (3) Specimens with a "P" prefix were received treated with Immunol and exposed to debris from the explosive expansion.

5-19

Table 5-3 COMPOSITIONS OF ALLOYS USED TO PREPARE MINI-U-SENDS (values in weight %)

Element Nb

+

N1 Cr Fe Ti Al Ta P Cu Co _ Other Alloy C 1 Mn S Inconel X-750 0.04 0.03 <0.01 0.004 72.57 15.60 7.10 2.60 0.70 1.01 - 0.01 0.03 -

0.23 No 0.038 0.86 0.40 0.003 4.30 i$'. 79 Ba1. 0.01 0.02 0.32 0.31 3.29 0.08 0.025 N 410 0.11 0.30 0.44 0.009 0.40 12.48 Ba1. - - - 0.017 - - 0.24 No 304 0.061 0.60 1.60 0.02 9.20 18.45 Ba1. - .

- 0.031 0.32 0.13 0.42 No 0.10 N "4

o 10.0 19.0 308L* 0.03 1. 0 2.0 0.03 to to sal. - - -

0.045 - - -

12.0 21.0 Inconel 600 0.06 0.22 0.17 0.007 76.05 15.40 7.92 - - - -

0.15 - -

Inconel 42 0.02 0.16 3.17 0.004 72.32 19.04 2.25 0.35 -

2.51 - 0.14 - -

Zirealoy 4- 0.016 0.10 0.20 1.64 Sn 0.13 0 (Ba1. Zr) e approsteete composition

l Table 5-4 ALLOY SUPPLIER, HEAT NO., AND FORM Heat No. or Heat Treatment Alloy Supplier Code Form Inconel X-750 Universal Cyclops Corp. Q902 Plug machined Pittsburgh, Pa. from bar stock 17-4 pH JOSLYN Stainless Steel, Heat No. 80581 Bar stock i

Fort Wayne, Inc. (2.5" dia) 410 Carpenter Technology, Heat No. 829985 1" plate Reading Pa.

304 Jessop Steel Co., Heat No. 30653 Plate Washington, Pa.

308L -- --

Wire Inconel 600 Williams and Co., Heat No. NX9349 Plate Pittsburgh, Pa.

Inconel 82 Huntington Alloys, Inc., Heat No. 7298D Wire Huntington, West Va.

Zircaloy 4 Data Proprietary - Stress annealed similar to B+W tubing.

4 5-21

Table 5-5 ALLOY HEAT TREATMENT AND MECHANICAL PROPERTIES Yield Tensile Rockwell Strength Strength Elong.,

Hardness kai kai in 2", I Alloy Heat Treatment Inconel X-750 1800*F/0.5 h + 1350*F/8 h + 1150*F/10 h C-38.4 17-4 pH 1900*F/1 h + 1100*F/4 h* -

410 1600*F/0.5 h + furnace cool to 1100*F** -

304 As Received - 41.1 84.0 66 Y 1150/7 h***

. U - -

308L - - -

Inconel 600 As Received (co'1d rolled, annealed B-80.0 47.0 91.0 45 and pickled)

Inconel 82 -

Zircaloy 4 Intermediate anneal 1250*F + final -

89 116 18 anneal 925*F Westinghouse anneals 3689 and 3690 Westinghouse anneal 3688 Westinghouse anneal 3687

l l

{ ,

r I

i Table 5-6 ALLOYS AND U-BEND CODING Coding of Alloy Mini-U-Bends Inconel K-750 Q-11 J

Q-12 i

I 17-4 pH A-1

' A-2

)

410 B-1 I B-2 304 C-1

)

i (1150 F/7 h)' C-2 308L Filler Metal D-1 on 304 (as required) D-2 Inconel 82 Filler Metal E-1

! on Inconel 600 E-2 i

j i

i b

! 5-23

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

Table 5-7  ;

LONG TERM CORROSION IEST CHEMISTRY SPECIFICATIONS Test Test No. 1 No. 2,3,4 Boron (H3B03 )* 2350 - 100 ppm B 2350 - 100 ppn B Lithium (LiOH)* 2.5 - 0.7 ppm Li 2.5 - 0.7 ppm Li Thiosulfate (Na2S02 3)** 0.05 .15 ppm SO4 ~~~~~~~~

Sulfate (Na 2SO4 ) --

.05 .15 ppm SO4 Chloride (Nacl) 0.05 .15 ppm C1 .05 .15 ppm C1 Fluoride (NaF) 0.05 .15 ppm F .05 .15 ppm F pH 5.0 - 7.5 5.0 - 7.5 Hydrogen 15-40 cc/kg 15-40 cc/kg Hydrazine (N24H) 2-10 ppm 2-10 ppm Oxygen < 10 ppb < 10 ppb

• Concentrations for each cycle are given below.

8*Specified as sulfate equivalent BORON LITHlUM CYCLE (ppm) (ppm) j Preconditioning 2350 50 2.2 - 2.5 HFT 2350 1 50 2.2 - 2.5 First Cycle 1200 1 20 2.2 - 2.5 Second Cycle 1000 1 20 1.7 - 2.0 Third Cycle 500 i 10 1.0 - 1.3 Fourth Cycle (which ends Tests 3 and 4) 100 1 10 0.7 - 1.0 [

t Fifth Cycle 100 10 0.7 - 1.0 l 1

Sixth Cycle (which ends Tests 1 and 2) 100 10 0.7 - 1.0 t i

5-24

l Table 5-8 Chemical Composition of Make-up Tank Solutions (Leak Rate Measurements)

Dissolved B Li F C1 S0 NH24 Conductivpty Oxygen 4 pH (umho em" ) (ppb) (ppm) (ppm) (ppm) M (ppm)

<10 490 1.0 0.05 0.05 0.05 2, Target 5.0 --

to tg to to to to Composition to 0.15 0.15 7.5 510 1.3 0.15 1p 4

~

Date Samples 35.8 470 0.88 <0.05 0.367 7/25/83 6.5 <5 0.121 9.f6 7/27/83 -- -- -- 474 0.88 <0.05 0.369 0.126 9.p6 l

l 5-25

6. OPERATING HISTORY The operating parameters for the long-term corrosion, peroxide cleaning, and leak rate experiments were specified by GPU-N to simulate expected operating parameters of the TMI-l steam generators. The experiments consist of maintaining pressurized flow of solution through the specimens while varying temperature and the applied load on the full-size specimens.

Four autoclaves have been used for the LTCT program. Tests 2, 3 and 4 contained specimens exposed to sulfate chemistry and Test I contained specimens exposed to thiosulfate chemistry. Autoclaves 3 and 4 had been operated in series for the peroxide experiment and have been converted into once-through long term corrosion apparatus for exposure of specimens exposed to the 500 hour0.00579 days <br />0.139 hours <br />8.267196e-4 weeks <br />1.9025e-4 months <br /> peroxide treatment.

6.1 Test Parameter Recording and Control 6.1.1 Temperature Proportional type controllers regulated current to autoclave i

heaters. The indicating thermocouple was placed in a well inserted through the head into the autoclave water. The control thermocouple J

was in contact with the autoclave OD within the space envelope generated by the band heaters.

l Typical temperature variation was +5'F. Temperatures were recorded daily.

6.1.2 Pressure Specimen ID and OD (autoclave) pressures were equal due to leaks in the specimen package. The pressure was developed and maintained with 6-1

a high pressure diaphragm pump and a mechanical back pressure regulator.

f The test system pressure was maintained 20 psig.

The bellows gas pressure used to maintain specimen load was controlled to within i 20 psig which is equivalent to about i 10 lb on the specimens. Since the response of both specimens in an autoclave was

-slightly different, due to slack in the loading system, total specimen load may have varied i 10 percent from specification.

6.1.3 Flow Rate Solution flow rates were typically 100 1 50 cc/hr. Some deviations occurred during temperature cycling; these were compensated for by adjusting the pumping rates where possible.

6.1.4 Record of Test Parameters Monthly tabulations of recorded temperatures, pressures and flowrates for Tests 1 through 4 are presented in Appendix 9.7. This appendix also contains plots of the measured temperatures and pressures for these tests.

6.2 Loop Cleaning and Preconditioning Upon the completion of construction of each autoclave loop system, a period of cleaning and sulfur preconditioning was undertaken prior to LTCT operations. The pre-operational system flushing and cleanup was accomplished by pumping high purity demineralized water from the MUT through the system with the autoclave at 6000F. During the cleanup, test samples were not placed in the autoclave with the result that the flushing process also cleaned the internal autoclave surfaces. The effectiveness of the hot water flush was determined by evaluating the results of periodic conductivity and chloride ion analyses.

The following values are typical of those found for the makeup water used during the flushing process: conductivity < 0.5 umho, Cl-6-2

< 1 ppb, F < 1 ppb, SO 2 =1 ppb. Flushing was terminated on Loop No. 2 when a Cl- concentration of 0.2 ppm and conductivity of 6 umho was achieved. When flushing was terminated on Loop No. 1 the following

~

concentrations in the loop effluent were measured: F~ = 1 ppb, Cl =

2-4 ppb, S0 = 9 ppb. The same procedure was followed for Loops 3 and 4 before the peroxide experiment.

During preconditioning, a length of stainless steel tubing was placed in the autoclave and fastened to inlet and outlet ports on the autoclave head. Preconditioning solution, therefore, flowed through this tubing and did not contact the autoclave internal surfaces. The

" preconditioned" stainless tubing was subsequently used to prepare the sample train used in the respective LTCT exposures.

Both autoclave loops were preconditioned at 600 F with solution identical to that used in the Test 2 HFT cycles. Flow of precondi-tioningsolutionwasmaintaineduntilaneffluentSOf~ concentration

> 90 percent of the influent value was achieved. Three to five days was required to precondition test systems.

6.3 Autoclave Loading Test specimen identification for each autoclave is shown in Table 6-1. Table 6-2 describes the further processing of the specimens.

It is an updated version of Table 4 in Reference 1. All C-rings and U-bends were placed in cans in series flow with the full size tubes. A typical package of specimens is shown in Figure 6-1.

6.4 Specimen Loads The total load applied to a tube specimen is the summation of the load applied by the bellows and the load resulting from the pressure differential across the tube wall. Since it was originally intended to operate each test system with a SP across the specimen walls, procedures were ' written which required that the bellows pressure be adjusted to compensate for changes in pressure across the tubing wall during thermal transients and, therefore, would maintain the sample load constant.

However, during heatup it was noted that the primary to secondary AP decreased more rapidly than anticipated and eventually became zero due to primary to secondary system leakage through defects in the test 6-3

specimens. During heatup the net effect of through-wall leakage and thermal expansion of the secondary fluid was the gradual elimination of the AP and establishment of a single phase (solid) secondary system.

Until the secondary system was solid, this required that the bellows pressure be increased,to maintain a constant sample load. But once the system was solid, specimen load was controlled solely by bellows load.

Controlling specimen load during cooldown became so experimentally difficult that it required almost continual monitoring and control.

This resulted f rom the f act that the leak rate through the tube defect was variable and insufficient to compensate for the contraction of water during cooldown.

A modification was therefore made to each of the four test systems which simplified the control of specimen load. The modification consisted of installation of a bleed line from the primary system to the j autoclave or secondary side. This line permitted the primary solution to fill the autoclave and maintain a solid secondary system at the same pressure as the primary system throughout the entire experiment.

Elimination of the AP across the tube permitted the specimen load to be controlled by only the bellows loading system.

6.5 Long Term Corrosion Experiments l Autoclaves were operated as long term corrosion experiments 1 through 4. The experiments consisted of a hot functional test (lift) of about one month duration followed by a series of six two month operational cycles for Loops 1 and 2 and four two month operational cycles for Loops 3 and 4. Solution chemistry was changed at the beginning of each cycle in accordance with Table 5-7. During each phase the system temperature and full size specimen loads were varied to simulate actual steam generator operating conditions.

The detailed test sequences for the HFT and operating cycles are presented in Appendix 9.1 and in 9.2, respectively. During heat up and while at temperature the full size specimen loads were maintained at 500 lb. At the beginning of each cool down to ambient, the load was increased to 1100 lbs and held there until the final temperature was 6-4

l reached. The load wassthen reduced to 500 lbs., except at the end of the cycle where it was reduced to 0.

Figure 6-2'is a stylized curve of the temperature vs. time regime for the HFT cycle of the GPU-N lead tests, and as such is an idealized representation of the cycle for the four autoclaves, Lead Tests 1 through 4 Figure 6-3 is also a stylized curve depicting the ideal thermal profile for all of the subsequent operating cycles of all GPU-N Lead Tests.

The departure of the temperature from the ideal curve was minimal in the ramping, cycling, and steady state stages of the HFT and F operating cycles.

Computer generated curves and tables for the actual operating parameters of Tests 1 through 4 for all HFT and operational cycles are presented in Appendix 9.6.

Water samples were withdrawn f rom the make-up tank and autoclave effluent af ter each new batch of make-up water was added (~ 3 weeks) and two weeks thereafter. ,

6.6 Autoclave Operational Variations ,

The first two autoclaves operated through the first cycle with little deviation from specifications. One general variation was the adjustment i of the test sequences to conform to a five day work week. For example, Step 6 of the operational sequence (see Appendix 9.2) requires 10 continuous days of temperature cycles. These cycles were interrupted during week ends. The test temperature at the end of a work week was maintained through the weekend. At the beginning of the next work week, cycling was reinitiated as prescribed in the test sequence.

Test 2 was started before a technique was developed for measuring specimen load from bellows pressure. During the HFT it is estimated that loads were actually 200 lbs low in the specimen. Also, r for this autoclave one bellows failed during the pressure increase f

6-5

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

preceding the cooldown to ambient for both the HFT and Cycle 1. After each bellows f ailure, the' system was opened, the bellows replaced and the remainder of the test continued according to the test specifi-cation. The net . effect of the bellows f ailure was loss of load during the cooldown from 600 to 1400F. The bellows f ailure did not occur until most of the load increase was achieved with the result that the tubes were subjected to most (but not all) of the high stress at 600 0F. The effect of this deviation from the test specification on the tube integrity can not be assessed.

Examination of the bellows indicated ID initiated stress corrosion cracking as the cause of the failure. Failure was, therefore, from the gas side and not a result of exposure to autoclave water.

Residual moisture and chloride contamination were suspected in the failed bellows. All bellows internal surfaces were subsequently washed in high purity water and thoroughly dried before use.

Minor deviations from specifications are recorded in daily record log books on permanent file in the Westinghouse Research Center '

Remote Metallographic Laboratory.

6.7 Leak Rate Experiment A small specimen of TMI #1 steam generator tubing with a through-wall defect was tested to determine the leak rate through the defect under various axial loads.

Prior to beginning leak rate measurements, the loading fixture containing the specimen with the through-wall defect was suspended from the autoclave head. The " secondary system" (consisting of the autoclave and the autoclave effluent sample cooler and back pressure regulator) and the " primary system" (consisting of the make-up tank, pump, tube specimen, sample effluent cooler and back pressure regulator) were filled with test solution.

6-6

i I

i i

i The pressure of both the primary and secondary systems was set at 2350 psi w'ith the respective back pressure regulator prior to heating the autoclave to 550*F. At temperature, the secondary system back pressure

( regulator was adjusted to 1175 psi. Under these conditions, the load 1 I due to the AP across tube wall balanced the compressive load applied by the turnbuckles thereby producing the zero load condition. Additional load was supplied to the specimen by increasing the bellows pressure to l

I the appropriate level.

4 A series of 7 primary-to-secondary leak rate measurements was made at

! axial loads between 0 and 1500 psi by collecting and measuring solution 1

i flow from the secondary system back pressure regulator. Each leak rate 1

l determination usually lasted 30 minutes with leakage volumes measured at five minute intervals. The test data from each run are presented in the i '

i Results Section 7.5.

j

[ 6.8 Chemistry Monitoring During the HFT and First Through Fourth Operating Cycles of Lead Test 1 I

During the performance of the various test cycles, analyses of MUT solutions and effluent solutions, which had passed through or over the test specimens, were routinely performed. The intent was to control l MUT chemical concentrations within specified limits and monitor effluent (

l solution levels to determine what changes may have resulted f rom -

l exposure to the test specimens. The results of these analyses would Provide documentation of the chemical composition of the test solutions l

during each of the exposure periods, i i MUT solutions were prepared as described in Appendix 9.3 (Section -9.3.2) f rom concentrated stock solutions which in turn were prepared as described in Appendix 9.3 (Section 9.3.1). MUT solutions i

i i 6-7 I

- - -,-n,- - -,~,---,,,--r ----,,-,----,r - - < - - , , , . . - ,- ,w -- ---,-.-,.n-- w- -~--,n -c-

l l

l were always prepared from stock solutions whose concentrations had been verified by chemical analyses. However, due to the time delay between sampling and analyses of MUT solutions, no adjustments were made in make-up tank compositions based on the results of chemical analyses of j MUT samples. In aost cases, make-up tank solutions were completely consumed prior to receipt of the results of chemical analyses on samples withdrawn shortly after their preparation.

The analytical chemistry results for samples collected from Lead Test 1 are given in Tables 6-2 through 6-6 for the HFT, first through fourth operating cycles, respectively. The data in these tables show l that no difficulty was encountered in maintaining either MUT pH or dissolved oxygen within control limits. Minor deviations in lithium and l boron target concentrations were observed during all cycles. These variations may have arisen partly from operational considerations between and during cycles.

Between each operational cycle, the MUTs were backflushed with deionized water and drained prior to filling with freshly prepared MUT i solutions. If the MUT had been incompletely drained following the flushing operation, the new NUT charge would be diluted by any unremoved flush water. The location of the drain valve on the MUT (in the side rather than the bottom of the tank) makes incomplete removal of flush

] water a probable event resulting in a decrease in both lithium and boron in some cases.

Likewise there was at least one operational variation which could have resulted in an increase in chemical concentrations of these species. After preparation, each MUT solution is sparged with inert gas to remove dissolved oxygen. If the sparging rate or length of sparging time varied between MUT preparations, concentration of MUT nonvolatile species may have resulted by loss of water vapor, carried off with the sparging gas. Either of these two events or some combination of these events may have occurred and caused the observed variations in targeted l MUT concentrations.

6-8 i

Minor difficulties in control of boron concentrations became apparent as the concentration and the corresponding control band for boron decreased. The relatively narrow control band for boron established at the lower nominal boron concentrations appears to be an unreasonably tight control band in the small volume test systems employed in this program.

Fluoride, chloride and thiosulf ate were to be controlled at low ppb levels in this test. Initially difficulty was encountered with control of the MUT fluoride concentrations. Experience in both Lead Test I and 2 showed that, although required volumes of the analytically verified fluoride stock solution were added to the MUT, low resulting fluoride concentrations were observed. This was attributed to adsorption of fluoride on the walls of the polyethlylene holding tank.

The practice of adding F directly to the stainless steel MUT during transfer of solution from the polyethylene holding tank was adopted to attempt to minimize adsorption, but this practice has proved inadequate in increasing MUT fluoride levels. Adsorption of fluoride on the stainless steel MUT walls is also thought to be occurring.

Some difficulty was also encountered in controlling chloride at the desired MUT levels. Although chloride levels in the MUT were within the targeted control band during the HFT cycle of Test 2, MUT chloride concentrations during the HFT and second operating cycle were frequently a factor of two high.

Although the targeted thiosulfate level in this test (0.0585 ppa) was only slightly above the limit of detection of thiosulf ate by the ion chromatographic analysis method, no thiosulf ate was detected in any MUT or, effluent samples. Although sulfate was routinely detected in effluent samples, the level of sulfate in these samples decreased with time during each cycle. The predicted sulfate concentration based on the thiosulfate input from the MUT should have been 40.1 ppm. It can not be determined whether the observed sulfate was derived fro.m thiosulfate or das simply a result of specimen (or specimen train) sulf ate contamination.

6-9

1 1

j Initial ef fluent samples were high in fluoride (HFT Cycle),

chloride and sulfate in each test cycle. Values for these species did 5 decrease with continued exposure to fresh MUT solutions and effluent 1

concentrations gradually approached those of the MUT solutions. .This is

! attributed to contamination of the specimens and specimen trains during l post exposure visual examinations. This contamination occurred despite strict compliance with operational procedures and techniques designed to minimize contamination. The highest effluent levels were observed in j the initial effluent sample taken during the HFT cycle. Since the full

! length tube specimens received no pre-test rinsing and since some specimens received surfactant treatment, these high initial effluent values j are not unreasonable.

Overall deviations f rom targeted concentrations have not been i great and ,are not expected to have a major impact on tube corrosion.

?

6.9 Chemistry Monitoring During the Fifth and Sixth Operating Cycles of Lead Test 1 Tabulations for the fifth and sixth operating cycles of Lead i

Test 1 are found in Tables 6-7 and 6-8. They list new data which was j acquired since the issurance of the second interim report and also repre-sent the concluding values for this test. It was ended on May 22, 1984.  !

j As discussed in Section 6.7 for the previous four cycles the only diffi-

~

culty in controlling the contaninent species within specifications was

~

j with the C1 and S203 levels. The discussion found in the previous section are also pertinent to the final two cycles.

i.

l 6.10 Chemistry Monitoring During the HFT. First Through Fourth Operating Cycles of Lead Test 2

] Tables 6-9 through 6-13 are tabulations of the analytical chemistry results for water samples withdrawn during HFT,,first through fourth operating cycles, respectively, of Lead Test 2. As in Test 1 (Section 6.7) some dif ficulty was encountered in maintaining Li+, B+, C1. F and SO 4 "Ilhin the targeted MUT. range for each of these species. The discussion found in Section 6.7 is also pertinent for the results of this test. The high 6-10 l

1'

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

~

initial effluent values for F , Cl", and SO ~4 observed early in each cycle are attributed to wash-off of these species frem specimen and specimen container surfaces.

6.11 Chemistry Monitoring During the Fifth and Sixth Operating Cycles of Lead Test 2 In Tables 6-14 and 6-15 a summary is found listing the analytical chemistry results for the final two cycles of Lead Test 2. They represent new data points, which have not yet been included in any of the previous reports.

As can be conciuded from the analysis for the last two operational cycles the chemistry control was right on target to maintain all species within specs. The only minor difficulty remained with the control of the

~

Cl level. The discussion found in Section 6.7 is also applicable to these final two cycles, which ended Lead Test 2 in May 1984.

6.12 Hydrogen Peroxide Experiment The hydrogen peroxide experiment was a 500 hour0.00579 days <br />0.139 hours <br />8.267196e-4 weeks <br />1.9025e-4 months <br /> experiment designed to simulate the proposed TMI-1 steam generator cleaning proce-dures. Samples exposed to this cleaning procedure were subsequently used in Lead Tests 3 and 4.

Solutions containing hydrogen peroxide were passed through a series of full size tube specimens and cans of U-bends and C-rings.

The recirculating system was regularly replenished with H22 0 to maintain the peroxide concentration in the specified control range.

Nominal operating parameter specifications for this experiment were:

6-11

?

Temperature , 130'F Pressure , 10 psig (from make-up tank overpressure)

Flow rate .

2 gallons /hr pH , 8.0 - 8.2 ,

Boron , 2350 ppa Lithium , 1.5-2.2 ppm H022 level , 15 - 20 ppm Full size specimen load , 500 lbs.

6.12.1 Loop Cleaning and Preconditioning

$ Cleanup and preconditioning of the loops used in the peroxide

! cleaning procedure was accomplished as described in Section 6.2. Each autoclave assembly was flushed with high purity deionized water, with the plumbing in the once-through mode. Water flushing of the first I

peroxide loop autoclave (Loop 3) commenced January 28, 1983 and was completed on February 3,1983; the flushing of the second peroxide loop j autoclave (Loop 4) began on February 7,1983 and was completed on February 9, 1983. The high purity water cleanup of the autoclave systems was followed by a sulfate preconditioning with the loop plumbing l remaining in the individual, once through configuration.

The primary function of the sulfate preconditioning was to attain a stable system " steady state", relative to the sulfate, in which 4

the sulfate concentration of the effluent is at or near the sulfate of l the influent solution. This was accomplished by exposing the tubing and system, exclusive of the GPU-N specimens, to a sulfate solution and analyzing the effluent. The sulfate analytical results for Loops 3 and 4 in the once-through cleaning and flushing operation are given in Tables 6-16and 6-17, respectively.

1 a e 6-12

~

. i Since there was interest in monitoring the loop sulfate level during the hydrogen peroxide experiment, care was taken during the clean-up and preconditioning of the loop systems to establish baseline sulfate values. Tables 6-16 and 6-17 present the results of sulf ate analyses obtained by ion chromotography for samples withdrawn f rom the loops during these operations. Sulfate greconditioning of Loop 3 was completed on February 9. The preconditioning of Loop 4 was completed on February 17, 1983.

6.12.2 Loop Operation with Peroxide Additions After preconditioning, Loops 3 and 4 were combined as shown in Figure 4-3 to form the closed loop system used during the perioxide cleaning. The specimens, as identified in Table 6-1, were placed in Autoclaves 3 and 4 and the MUT filled with 501 of a solution containing 2350 ppa B as boric acid and 2.1 ppm lithium as lithium hydroxide.

Af ter the MUT was sampled to determine the baseline Sof' level (see Table 6-17), one liter of MUT solution was flushed through the system (specimens remained by-passed) and removed via the effluent sampling line.

A sample of this initial flush solution was also retained for analysis (See Table 6-17 ).

Additions of ammonium hydroxide and sodium sulfate solutions were made to adjust the MUT pH to 8.2 and increase the sulfate concen-tration to a value comparable to that used during loop preconditioning.

These additions were also made with the test specimens by-passed.

6-13

Because a " primary-to-secondary" leak at the tube collar weld was detected during the leak checking (which is part of the specimen assembly procedure) a drain line was connected from autoclave 3 to the i HUT. This drain line prohibited the autoclave pressure from gradually increasing to that of the primary system and, thereby, significantly simplified operation of the specimen loading fixture by eliminating the need to f requently adjust gas pressure in the bellows. This drain line

remained open to the MUT throughout the entire peroxide cleaning procedure.

The H 022 injections into the circulating system were started by discrete manual introduction at hourly intervals. ..Later, an automatic peroxide injector was added to the system to allow routine metered peroxide addition to the system.

A summary of the changes made to the apparatus for increased efficiency or because of unforeseen circumstances is given in Table 6-18.

The average daily peroxide concentration of the solution in the make-up tank, as well as the pH of this solution, is reported in Table 6-19; the daily peroxide usage is tabulated in Table 6-20 All of the pertinent peroxide data listed in Tables 6-19 and 6-20 are plotted in Figures 6-4, 6-5 and 6-6.

4 It should be noted that in order to maintain the peroxide concentration in the make-up tank (MUT) within the selected limits, the 1

peroxide additions (or deletions) were both continuous and discrete; i.e., the addition of the peroxide was generally accomplished with the automatic injector system, with additional manual injections if the HUT peroxide concentration was too low. Conversely, if the MUT peroxide

concentration began to increase over the target value, the injector was turned off for a predetermined length of time. Because of this distinction, the average rate of peroxide addition was determined by dividing the weight of peroxide added in a given period (in all but the first and last cases, one day) by the number of hours in that period.

6-14

The scatter in the data for the weight of peroxide added (concentration) and the average weight of addition for the first 90 hours0.00104 days <br />0.025 hours <br />1.488095e-4 weeks <br />3.4245e-5 months <br /> can be attributed to the learning process of the operators.

This learning process is graphically illustrated in Figure 6-4: as the skill of the operators increased, the range of values of the average daily MUT peroxide concentration decreased. After 150 hours0.00174 days <br />0.0417 hours <br />2.480159e-4 weeks <br />5.7075e-5 months <br /> of operation, there was a gradual decrease in the amount (and average cate) of peroxide addition needed to maintain a 15 ppm hydrogen peroxide concentration in the HUT (Figure 6-5). This decrease in the amount of H0 2 2 which was added can most probably be attributed to the gradual decrease in volume of solution in the loop caused by sampling.

f 6.12.3 Chemistry Monitoring During the Peroxide Experiment Daring the entire 500 hour0.00579 days <br />0.139 hours <br />8.267196e-4 weeks <br />1.9025e-4 months <br /> peroxide exposure control of chemistry was very good. Figure 6-6 shows that the syst em pit remained essentially constant at pH 8.2. Baron and lithium concentrations showed some minor variation which is presumed to be due to the normal fluxuation in values resulting f rom the analysis of these species and does not reflect any ef f ect of peroxide additions.

Peroxide concentrations initially showed some variation f ram the 15-20 ppm specification due to the insdequacy of manusi additions to compensate for consumption rates. Following installation of the i

peroxide injection system, the observed sprend in peroxide concentration l

values was narrowed significantly (See Figure 6-4).

l r

The analytical chemistry data obtained by analysis of the solutions withdrawn f rom the loop during the peroxide exposures are presente.1 in Table 6-21 During the first three days of exposure to peroxide containing solutions, the sulfate concentration in the effluent solutions gradually increased. Although the refilling of the HUT with fresh solution on the fourth day of testing (which was necessary due to solution lose resulting f rom the events documented in Table 6-19) caused l

l ,

a temporary reduction in the ef fluent sulf ate concentrations (simply by l

l 6-15

dilution) effluent sulfate values continued to increase through the first eight days of testing before stabilizing at ~ 300 ppb af ter 200 hours0.00231 days <br />0.0556 hours <br />3.306878e-4 weeks <br />7.61e-5 months <br /> of exposure. Although the observed increase in ef fluent sulf ate may have been due to oxidation of lower oxidation state sulfur i containing species on tube surface or to the release of sulfate from the network of intergranular attack comprising the tube def ects, the possibility that the observed increase in ef fluent sulfate was due to contamination during the preparation of C-rings and U-bends or during assembly of the full length tube specimens can not be discounted.

The inaccuracies involved in estinating the volumes of solution lost during the unexpected systes leaks of February 25 and 26 (see Table 6-18) make any attempt at a material balance for sulfate, at best, crude. Nevertheless, material balance calculations were nede which show that approximately 17 og of SOf" or approximately 7 og of S, in excess of that intentionally added to the loop in NUT solutions, was moved from sample train assemblies during the peroxide exposures.

6.13 Chemistry Cyclen Monitoring of Lead Tent 3During the HFT. First and Second Operating and 4__

Tables 6-23, 6-24. and 6-25 are tabulations of the analytical chemiatry results for water samples withdrawn during HFT, first and accond operating cycles, respectively, of Lead Test 3. Tables 6-26, 6-27 and 6-28 show the results of Lead Test 4 for the HFT, first and second operating cycles.

As in Tent 1 and 2 (Section 6.9) some dif ficulty was encountered in maintaining Li+, CL", F' and MUT concentrations within the targeted HUT range for each of those species.

The dincussion found in Section 6.8 is also pertinent for the results of this test.

The HUT lithium concen-trations for the HFT cycle and operational cyclen 1 and 2 for Tests 3 and 4 were consistently low by a small factor.

Sulfato concentrationn were--for the most part, except for an occasional excursion--very close to the specified control band.

6-16

F r

6.14 Chemistry Monitorinn During the Third and Fourth Cycles of Lead Test 3 and 4 The results of the chemical analyses of the samples withdrawn from the final two cycles 3 and 4 of Lead Test 3 and Lead Test 4 are presented in Tables 6-29 and 6-30, and 6-31 and 6-32, respectively.

This information is new and had not been included in either the 1st i or the 2nd interim reports. Chemistry monitoring during this time

~

period was very successful and aside from the somewhat high C1 and ,

~

low F icvels it followed the specifications satisfactorily.

1 overall it is felt that the chemistry variatione are not signifi-cant enough to have a major impact on the outcome of the metallographic examinations of the C-rings, U-bends and full size tubes.

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6-18 1

1 .- _ _ - _ _ _ _ _ _ _ _ _ _ - - _ _ - - _- _ _---_ - - -_..- -__ - - .-. - _ _ _ - .

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t i I I I I I I t

0 1 2 3 4 5 6 7 8 Cycle Time (H) i 700 - Temperature

' -- - Cycle A

600 C

2 500 -

] '

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1. 0 -

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]300 FT Cycle Add NH NH 200 -

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• 100 -

2 l

0 -*l ! = ' ' '

10 20 30 #

0 Time (days) 4 Figure 6-2. Stylized HFT Curve 6-19

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. Figure 6-5. Estimated H 022 Consumption Rates

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Table 6-1 AUTOCLAVE SPECIMEN LOADING C-Ring Full-Size Te st No. Tube Original Replacement U-Bend s 1 A13-63 1A1 -

(11-18 15/16)* 1A2 2B5 after HFT 1A3 after C cle 4 1B5 after cle 5

, A24-94 181 184 after C cle 1

) (19 5/16-25 7/15) 182 IDI 1D5 after Cycle 2 1D6 after Cycle 3 ID2 2A1 2B1 2D1 1El IE7A after Cycle 3 lE2 lE3 2 B16-22 2A2 1A5 after HFT -

l (52-59) 2A5 af ter Cycle 4 A88-7 2A4

-(2-9 3/4) 2B2 2B4 af ter Cycle 1 1D8 after Cycle 5 3

2D2 ID7 after Cycle 3 2D3 1A4 183 1D3 j 1E4 1ES lE8A after Cycle 3 IE6 6-24

_.,c . - - _ _ _ _ . _ -y . ,. . - _

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

l' Table 6-1 (continued)

C-Ring Full-Size Test No.- Tube Original Replacement U-Bends f

3 A16-69 PIAL Removed after H22 0 Run All (6 1/2-12 1/4) PIA 2 Removed af ter Cycle 1 l

i PIA 3 Removed after Cycle 2 PIA 4 Removed after Cycle 4 PIA 5 Removed after Cycic 4

, P2D1 Removed after Cycle 3 1

i P2D2 Removed during Cycle 3 for Auger P2A1 Removed after H 022 Run P2A2 Removed after HFT P2A3 Removed after Cycle 1 l

P2A4 Removed after Cycle 3 P2A5 Removed after Cycle 4 PIDI Removed after HFT PID2 Removed after Cycle 2 i

P1D3 Removed after Cycle 4

PID4 Removed after Cycle 4 P1D5 Removed after Cycle 4 4 A24-94 (36-42)

I B94-27 (4 1/2-10 1/2) l 4

i i

i 1

• Specimen reduced in size before start of test 1

6-25 i

l

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

Table 6-2 C-RING REPLACEMENT SEQUENCE CYCLE HFT 1 2 3 4 5 6 Loop #1 1Al*

• dcored l Auto- lA2* 2B5* 4 1A3 y l clave #31 l

1Bl*  ; 1B4*

• 1B5*

1B2* m btored r 1Di* i 1D5* 1D6 m 1D2 Stored i 2Al* m 2B1 Stored f

2D1* t 1E/A lEl* .

V, Stored ,

, i e i lE2* 4 l

l 1E3* s f

Loop #2 2A2* 1AS* St red

2A5 Auto- 2A4* '

clave #29 2B2*

2B4* l 2B3 Stored y 2D2* ., 1D7 Mrnrod -

2D3* s f

lA4* m f

IB3*

1D3 Stored s W

lE5*  ; g lE8A Renrod y lE6* ,

6-26

Table 6-2 (cont. )

HFT 1 2 3 4 Loop #3 PlA2*  ;

Auto- PlA3* l clave #20 PlA4* >

P1AS* >

PIDi* j PlD2* l PlD3 Starad >

P1D4 Stored y PlDS Stored y P2A2*

I P2A3* ,

i P2A4* i.

P2A5* s 1

l P2Di* l P2D2 i y, x ,x x ,1 ?( )

Removed for Auger Analysis PlA1)

P2A1 Removed after H022Exposure i

• Metallography reported l

l I

l l 6-27

Table 6-3 ANALYTICAL DATA FOR TEST l-HFT CYCLE I.i 4 NH24 S023 TIN) D.O. 14 F C1 i SOLRCE pil [pwho\ (PIN) (PIN) (PIN) (PlW) (PlW) (PlW) (PIM) (PIN)

\cm )

5.0 2.2 2300 0.05 0.05 2 j TARCET MUT to <0.010 to to to to -- to 0.0585 i CHEMISTRY LEVELS 7.5 2.5 2400 0.15 0.15 10 DATE TAlEN 1

11/2/82 >Sfr 6.5 40 <0.005 2.16 2323 0.075 2.22 0.183 0.053 <0.05 NEK MJr EFF 2.21 2332 0.972 58.45 0.908 0.040 <0.05 11/3/82

• 2.21 2358 0.06 0.436 0.202 0.086 <0.05 j 11/8/82 EFF 4

=

i 11/10/82 EFF 2.34 2359 0.06 0.282 0.181 0.086 <0.05 11/12/82 D81T 5.6 60 (Aln) 2.28 2352 0.06 0.292 0.178 2.00 <0.05 IEW Mfr OPE.N TO ADOSPIEltE 11/23/82 EFF 1.81 2519 <0.05 0.399 0.168 2.50 <0.05 1

504 equivalent = 0.05 to 0.15 PfM.

1 i

t

Table 6-4 ANALYTICAL DATA FOR TEST 1-IST OPERATING CYCLE 3

I.i B F C1 (TNil 11. 0 .

(PlN) (PlW) (PfW)

(PlW) (PIN) (PfM) , (PAN)

N Pil 9 (PIN) __

a '

2.2 1180 0.05 0.05 2.0 0.0585(Ash 2Sy03*

5.0 to -- en T w ET MUT <0.010 to to to to 10

• mralsvay t rvrt c ,

'7.5

~

2.5 1220 0.15 0.15 <

3 i.

DATE. TAKEN ,

a- <0.05 0.198 0.173 0.698 <0.05 2.65 1315 n '_N- mfr 6.08 .58 <0.002 v 12/22/82 <0.05

.- ~

'~

2.64 1249 40.05 0.232 0.064 0.041 12/28/32 DT ,

c'

<0.05 Ofi95 0.129 0.046 <0.05 2.72 1274 r ~ 12/29/82

- 17 7 'l -

<1.05 0.161 0.135 0.321 <0.05 7

Mrr 'd.13 50 <0.005 2.56 1217 ~ u

% 1/04/83 ,

<0.05 s- '

1.83 1260 <0.050 0.236 0.158 8.2

+ 1/13/83

~'

DT ,.

s

<0.050 0.223 0.064 4.5 <0.05

,1.% 1258 1/25/83 DT b.05Inefill l '

< .'00 5 1.85 1253 ,1 0 05C 0.2 15 0.064 9.8 MFr 6.13 52 1/26/83 f2.20 1735 b.050 0.141 0.026'<0.1 0; > - 2/03/83 DT ',

o,ggie.' .

<0.050 0.132 0.050 10.6 Inefill 6.03 53 <.005 2.11 1215 2/11/83 Md.' 0.053**

. ~

3.95 1203 <3.050 0.137 0.028 <0.1 f 2/23/83 DT 0.031**

2.15 1243 0.088 f

.3/02/83 DT 1246 0.120+

• • c Concentrator Co164mn

• Repeat Analysis i

l Table 6-5 -

ANALYTICAL DATA FOR TEST 1-2ND OPERATING CYCLE SO4 NH24 S023 F C1

11. 0 . I.i H .

(PlW) (PIN)

(11N) (PIN) (PIN) (PIN) (PlN) pil y sho_ (11N)

S0lmCE (CONil 0.05 0.05 2 0.0585 1.7 980 as 5.0 eo eo to -- to

<0.010 to 10 Na223 80 TARGET MI!T to 2.0 1020 0.15 0.15 CHEMISTRY LEVELS 7.5 DATE TAlEN <0.05

<0.005 1.71 1015 < 0.05 0.226 0.131 7.15 Bar 7.10 44.5 0.108+

3/4/83 <0.05 1.60 , 979 <0.05 +0.933 0.319 0.82 3/4/83 DT 0.340 i 0.3664 8 <0.05 1.75 1023 <0.05 0.223 0.061 <0.01 3/9/83 57 0.092+

<0.05 0.227 0.114 8.30 <0.05' MK 6.25 - <0.005 1.70 1028 3/21/83

<0.01 0.302 0.038 <0.01 <0.05 1.81 1040 3/23/83 EFF

<0.01 0.296 0.033 0.02 <0.05 1.52 1042 4/16/83 EFF

<0.01 0.274 0.056 16.5 <0.05 6.07 38 <0.005 1.71 1046 4/18/83 MUT 1030 <0.01 0.287 0.028 0.02 <0.05 EFF 1.62 4/23/83

+ Duplicate Analysis

1. Recheck 6/17/83

• GPU Designation

=

Table 6-6 ,

l ANALYTICAL DATA FOR TEST I -- 3RD OPERATING CYCLE l l

COND Cl SO4_

NH24 S0 23 DATE' u mho D.O. Li B F TAKEN SOURCE pH cm (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) ~(PPM)

TARGET MUT 5.0 (0.010 1.0 490 0.05 0.05 2 CHEMISTRY LEVELS to to to to to --

to 0.0585(As Na223 80) 7.5 1.3 510 0.15 0.15 10 6/27/83 MUT 6.31 32.4 ' <0.005 0.95 510 (0.05 0.194 0.027 8.56 <0.05 0.90 496 (0.05 0.194 0.027 8.95 <0.05-6/29/83 MUT 6/29/83 EFF 0.95 498 <0.05 0.295 0.466 <0.02 <0.05 6.53 33.2 <0.005 .l.06 472 <0. 05 ' O.292 0.030 8.1 <0.05 7/8/83 MUT 1.40 494 <0.05 0.284 0.033 7.9 <0.05 7/13/83 NUT 1.06 461 <0.05 0.296 0.037 <0.01 <0.05 7/13/83- EFF 0.97 495 <0.05 0.457 0.122 <0.02 <0.05 7/27/83 MUT EFF 0.96 499 <0.05 0.371 0.035 <0.02 <0.05 7/27/83 8/10/83 ' MdT 6.46 36.7 0.0075 1.01 476 <0.05 0.212 0.030 9.32 "QNS"*

8/10/83 EFF. 0.97 483 <0.05 0.225 0.022 0.213 "QNS"*

8/24/83 MUT 1.07 441 <0.05 0.2?4 0.030 7.23 <0.05 8/24/83 EFF 1.08 474 <0.05 0.228 0.018 0.005 (0.05

• Quantity not sufficient for analysis

Table 6-7 ANALYTICAL DATA FOR TEST 1 -- 4TH OPERATING CYCLE SO NH24 S0 23 DATK uao D.O. Li B F C1 4 TAKEN SOURCE pH cm (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) (PPM)

TARGET MUT 5.0 <0.010 0.7 90 0.05 0.05 2 to 0.0585(As Na280 CHEMISTRY LEVELS to to to to to 2 3) 7.5 1.0 110 0.15 0.15 to 9/20/83 MUT 6.94 25.8 <0.005 0.73 127 <0.05 0.156 0.051 8.63 9/26/83 MUT 0.65  !!3 <0.05 0.153 0.047 8.75 9/26/83 EFF 0.66 121 <0.05 0.198 0.072 <0.01 10/3/83 MUT 6.89 25.4 <0.005 0.62 112 <0.05 0.153 0.100 9.42 10/11/83 MUT 0.56 115 <0.05 0.161 0.103 9.39 10/11/83 EFF 0.67 116 <0.05 0.782* 0.212 0.03 .

[

10/19/83 10/19/83 MUT EFF 0.55 0.55 113

!!3

<0.05

<0.05 0.173 0.193 0.098 0.102 9.49 0.04 10/24/83 MUT 6.78 25.7 <0.005 0.82 93 <0.05 0.142 0.050 3.25 11/2/83 MUT 0.82 90 <0.05 0.139 0.045 2.09 11/2/83 EFF 0.85 90 <0.05 0.185 0.096 0.238

!!/16/83 EFF 0.831 103 <0.05 0.188 0.039 0.011 <0.05 11/15/83 MOT 7.08 25.7 <0.005 0.822 100 <0.05 0.331 0.035 9.40 <0.05 11/16/83 MUT 0.842 99 <0.05 0.234 0.078 7.37 <0.05 11/30/83 MUT 0.832 100 <0.05 0.313 0.031 9.59 <0.05 11/30/83 EFF 0.819 102 <0.05 0.236 0.038 0.011 <0.05

• bellows leaked - repair

- .-. . _ _ . - . . . . _ _ _ _ . _ _ _ _ _ _ _ _ . _ _ . . , _ _ _ ._m. __ _ . . _ . _ . _ _ . _ . - m _ . . _ . . .

Table 6-8 Analytical Data for' Test 1-5th Operating Cycle COND.' 0 H 80 23 D.O. Li 5- F C1 4 24 DATE. y mho (PPM) (PPM) (PPM) (PPM) (PPM) (PPM)

TAKEN SOURCE pH i cm (PPM) (PPM) l 2.0 5.0 < 0.010 0.7 90 0.05 0.05

• TARGET MUT to to to to -- to 0.0585(As Na $23 0)

CHEMISTRY LEVELS to 0.15 10 7.5 1.0 110 0.15 0.827 104- < 0.05 0.274 0.099 9.60 < 0.050 12/13/83 MUT 7.07 26.0 < 0.005 0.813 103 < 0.05 0.258 0.165 0.015 < 0.050 '

12/15/83 EFF 0.837 100 < 0.05 0.254 0.089 9.08 < 0.050 12/15/83 MUT

< 0.005 OL824 103 < 0.05 0.137 0.041 8.44 < 0.050 12/27/83 MUT 7.05 25.8 0.915 101 < 0.05 0.285 0.030 0.010 < 0.050 .

12/28/83 EFF m 103 < 0.05 0.219 0.039 0.291 < 0.050 0.816 12/28/83 MUT 0.76 87 < 0.05 0.159 0.016* 0.006 < 0.050 1/11/84' EFF 0.78 87 < 0.05 0.152 0.020* 7.04 < 0.050 1/11/84 MUT 25.5 < 0.005 0.79 87 < 0.05 0.209 0.026* 9.99 < 0.050 1/17/84 MUT 7.11 0.82 87 < 0.05 .0.175 0.029* 0.006 < 0.050 ,

1/26/84 EFF 0.78 87 < 0.05 0.191 0.038* 9.35 < 0.050 1/26/84 MUT 25.6 < 0.005 0.76- 84 < 0.05 0.147 0.035 8.74 < 0.050 2/3/84 MUT 6.80 0.82 84 < 0.05 0.198 0.013 0.010 < 0.050 2/8/84 EFF O.81 84 < 0.05 0.183 0.108 8.36 < 0.050 i 2/8/84 MUT' t

'

• Concentrator Column Analysis 1

4 1

Table 6-9 Analytical Data for Test 1-6th Operating Cycle i

'COND.' 80 I DATE u mho D.O. Li B F C1 4 2"4 23 TAKEN SOURCE pH i cm (PPM) (PPM) (PPM) (PPM) (PfM) (PPM) (PPM) (PPM)

TARCET MUT 5.0 < 0.010 0.7 90 0.05 0.05 2.0 CHEMISTRY LEVELS to to to to to --

to 0.0585(As Na,S

~230 ).

i

~

7.5 1.0 110 0.15 0.15 10

< 0.005 0.84 99 < 0.05 0.379 0.158 3.17 < 0.05 3/13/84 MUT 6.38 25.7 0.85 103 < 0.05 0.401 0.261 < 0.05 < 0.05 3/14/84 EFF 0.85 103 < 0.05 0.372 0.149 3.17 < 0.05 3/14/84 MUT 26.0 < 0.005 0.86 95 < 0.05 0.364 0.169 4.46 < 0.05 3/21/84 MUT 7.07 0.84 99 < 0.05 0.328 0.042 < 0.05 < 0.05 i 3/28/84 EFF 0.87 107 < 0.05 0.320 0.074 7.66 < 0.05

[ 3/28/84 MUT

< 0.005 0.82 98 < 0.05 0.332 0.102 5.90 < 0.05

" '4/5/84 MUT 7.01 25.1 0.82 99 < 0.05 0.361 0.043 0.08 < 0.05 4/12/84 .EFF 0.82 99 < 0.05 0.316 0.084 6.72 0.071 4/12/84 MUT 7.22 24.8 < 0.005 0.83 97 < 0105 0.311 0.069 7.06 < 0.05 4/19/84 MUT 0.84 98 < 0.05 0.319 0.029 < 0.05 < 0.05 4/25/&4 EFF 0.85 100 < 0.05 0.325 0.054 7.92 < 0.05 f 4/25/84 MUT 7.45 25.6 < 0.005 0.86 102 < 0.05 0.254 0.136 4.5* < 0.05 5/3/84 MUT 0.85 100 < 0.05 0.215 0.024 0.03* < 0.05

'$/10/84 EFF 0.86 101 < 0.05 0.206 0.124 4.1* < 0.05 l 3/10/84 MUT 5/18/84 MUT < 0.005 0.82 100 < 0.05 0.249 0.129 5.8* < 0.05

• Concentrator Column Analysis k

l s

- _. . . _ _ _ _m . _ . . _ _ _ - . , _ _ _- _ _ . . _ _ _ _ _ _ _ . . . _ _ - . _ . _ _ _ _ . _ _ _ _

"~

Table 6-10 A ANALYTICAL DATA FOR TEST 2-HFT CYCLE

• 1.,

4 N II24 S023 CONil 11. 0 . 1.i H I: C1 SOUltCli pil [ p uho \ (l'IN) (PIN)* (PIN) (PIN) (PIN) (l'IN) (PlW) (PlW)

\ cm ) >

5.0 2.2 2300 0.05 0.05 0.05 2 TARGET Hl:T to <0.010 to ta to to to !o -

CliEMISTRY T EVFI.S 7.5 2.5 2400 0.15 0.15 0.15 10 DATE TMIN Research 10/19/82 m 5.73 42 <0.005 2.2 2395 0.02 0.06 0.115 " evidence" Analysis W^II* II m 1.90 0.08 0.08 0.08 2.75 '

10/22/82 2341 Analysis

-- SPIl@ M Willi F,Cl-

'O 10/25/82 MLfr 1.97 2296 0.06 0.118 0.388 5.27 10/25/82 DT 2.10 2303 2.38 1.23 0.511 0.15 -

10/28/82 MLFr 2.01 2315 0.041 0.102 0.214 0.44 <0.05 - .

10/28/82 DT 1.98 2305 0.47 0.47 0.24 0.018 2.00 0.073 #

11/2/82 M 5.6 38 (Air) 2297 0.100 0.234 0.76 <0.05 Refill Open to Ait 11/11/82 .M 2.07 2350 0.06 0.155 0.220 0.193 <0.05 11/11/82 DT 2.07' 2348 0.05 0.248 0.236 0.079 <0.05 i

'l L

i

Table 6-11 ANALYTICAL DATA FOR TEST 2-IST CYCLE 1.i in F. Cl. 4 Nzil4 S023 awl) 11. 0 .

SOUltCE pil (PIN) (PAN) (PIN) (PIN) (l'IN) (PIN) (PlH) (PlW)

('yahoem TARGEI MCT 5.0 2.2 1180 0.05 0.05 0.05 2 CHDilSTRY LEVELS to <0.010 to to to to to to --

7.5 2.5 1220 0.15 0.15 0.15 10 DAlli TAKDI 12/3/82 WI 2.07 1310 <0.05 0.323 0.171 0.02 E I MlTT 6.5 40 10005 1.94  !!!9 <0.05 0.2% 0.140 3.24 12/10/82 //2 12/10/82 EFF 1.95 1281 <0.05 1.60 0.245 0.05 12/10/82 EFF 1.88 1185 <0.05 0.538 0.200 <0.01 12/21/82 MJr 6.03 52 -<0.005 2.16 1205 <0.05 0.146 0.039 0.005 REFILL MJr e 0.136+

EFF 2.25 11 % <0.05 0.148 0.037 0.005 6 12/23/82 1/6/83 EFF 2.14 1209 <0.05 0.163 kfikI 0.012 ,

1/11/83 Mir 6.00 67 10005 1.87 1205 <0.05 0.217 0.098 4.6 <0.05 REFILL 1/26/83 EFF 1.93 1187 <0.05 0.236 0.097 <1 <0.05 2/1/83 WT 6.10 51 <0.005 2.15 1214 <0.050 0.138 0.160 8.0 REFILL 0.179 2/8/83 El'F 1.95 1204 <0.050 0.147 0.145 <0.1 0.152 2/16/83 EIT 2.30 1203 <0.050 0.151 0.206 0.11 0.221 2/17/83 EIT 2.29 1203 <0.050 0.127 0.179 3.6 0.197

• Concentrator foltsan.

+ Repeat Analysis

Table 6-12 ANALYTICAL DATA FOR TEST 2-2ND OPERATING CYCLE 4 2 3 1.i il F C1 (PIM)

LINil 11. 0 .

(PIM) (PIM) (PiW)

(PIN) (PIN) (PIN)

SOURCL pil [ p whq \ (PIN)

\ cm ) 0.05 0.05 0.05 0.05 1.7 980 to 5.0 to to to to t t 0.15 0.15 0.15 0.15

<0.010 .2.0 1020 TARGET NUT 7.5 CHEMISTRY LEVELS 0.40 New DATE TAKEN <0.05 0.242 0.171

<0.005 1.48 998 MUT 6.50 70 2/27/83 <0.05 0.236 0.283 0.28 .

1.47 990 DT 2/28/83 <0.05 0.236 .135 0.22 6.17 33 <0.005 1.76 1026

).142 Refill ML7F i 3/8/83 .17588 .

w

<0.05 0.227 0.164 f0.02 1.70 1019 3/9/83 DT 0.16688)

<0.010 0.279 0.130 <0.01 .

1.72 1060 3/23/83 DT

<0.010 0.286 0.121 <0.01 1.79 1024 4/6/83 DT

<0.010 0.276 0.119 12.41

<0.005 1.72 1037 M7r 6.24 -

4/14/83 0.111 0.02 1.74 1037 <0.010 0.282 EFF 4/20/83 .

14 lon Chrmatography Ecop

Table 6-13 ANALYTICAL DATA FOR TEST 2 -- 3RD OPERATING CYCLE COND Cl 80 4 NH24 S0 23 DATE p mho D.O. Li B F TAKEN SOURCE pH cm (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) (PPM)

TARGET MUT 5.0 1.0 490 0.05 0.05 0.05 2 CHEMISTRY LEVELS to <0.010 to to to to to to --

7.5 1.3 510 0.15 0.15 0.15 10 6/24/83 MUT 6.38 39.0 <0.005 0.91 493 <0.05 0.194 0.138 1.12 <0.05 6/29/83 MUT 0.89 496 <0.05 0.202 0.145 0.10 <0.05 6/29/83 EFF 0.99 512 <0.05 0.249 0.151 0.03 <0.05 7/7/83 MUT 6.40 34.3 <0.005 1.06 457 <0.05 0.289 0.141 8.4 <0.05

, i' 7/13/83 Mur 1.06 474 (0.05 0.290 0.133 7.5 <0.05 7/13/83 EFF 1.11 465 <0.05 0.347 0.398 0.2 <0.05 7/25/83 MUT 6.48 35.8 <0.005 0.88 470 <0.05 0.367 0.121 9.36 <0.05 7/27/83 MUT 0.88 474 <0.05 0.369 0.126 9.46 <0.05 7/27/83 EFF 0.89 465 <0.05 0.377 0.122 9.64 <0.05 7/29/83 EFF 1.09 485 <0.05 0.217 0.123 5.93 "QNS"*

(Shutdown)

• Quantity not sufficient for analysis

Table 6-14 ANALYTICAL DATA FOR TEST 2 -- 4TH OPERATING CYCLE COND SO 4 NH 24 S0 23 p mho D.O. Li B F CL DATE (PPM) (PPM) (PPM) pH cm (PPM) (PPM) (PPM) (PPM) (PPM)

TAKEN SOURCE 5.0 <0.010 0.7 90 0.05 0.05 0.05 2 TARGET MUT to --

to to to to to CHEMISTRY LEVELS to 0.15 7.5 1.0 110 0.15 0.15 10 7.01 25.8 <0.005 0.74 123 <0.05 0.153 0.115 1.04 9/20/83 MUT 7.01 0.59 109 <0.05 0.152 0.108 9/26/83 MUT 0.02 EFF 0.59 109 <0.05 0.550* 0.188 9/26/83 8.15 MUT 7.09 30.4 <0.005 0.59 110 <0.05 0.150 0.085 10/3/83

- 0.51 115 <0.05 0.241 0.063 8.96 10/11/83 MUT EFF 0.53 108 <0.05 0.176 0.048 0.03 10/11/83

<0.05 0.162 0.059 9.06 10/19/83 MUT 0.55 111 f[*

i 10/19/83 EFF 0.58 til <0.05 0.169 0.042 <0.01 MUT 6.79 25.5 <0.005 0.52 110 <0.05 0.142 0.100 8.67 10/20/83 MUT 0.81 93 <0.05 0.135 0.095 5.97 11/2/83 EFF 0.83 87 <0.05 0.148 0.116' 5.87 ,

11/2/83 MuT 6.76 26.0 <0.005 0.848 97 <0.05 0.311 0.190- 8.64 <0.05 11/9/83 0.830 102 <0.05 0.148 0.118 0.068 <0.05 11/16/83 F.FF 0.839 99 <0.05 0.241 0.170 8.59 <0.05 11/16/83 MUT EFF 0.830 102 <0.05 0.210 0.082 0.014 <0.05 11/30/83 0.823 100 <0.05 0.291 0.066 9.74 <0.05 11/30/83 MUT

• long shutdown

Table 6-15 Analytical Data for Test 2-Sch Operating Cycle COND.* H 24 S0 23 p sho D.O. Li B F C1 4 DATE (PPM) (PPM)

(PPM) (PPM) (PPM) (PPM) (PPM) (PPM)

TAKEN SOURCE 'pH i cm

< 0.010 0.7 90 0.05 0.05 0.05 2.0 TARGET MUT 5.0 to to to to to to CHEMISTRY LEVELS to 0.15 10 7.5 1.0 110 0.15 0.15 98 < 0.05 0.289 0.236 1.56 < 0.050 7.08 25.7 < 0.005 0.826 12/13/83 MUT 0.802 100 < 0.05 0.164 0.116 0.075 < 0.050 12/15/83 EFF 0.817 100 < 0.05 0.219 0.161 4.43 < 0.050 12/15/83 MUT

< 0.050 0.843 100 < 0.05 0.287 0.226 10.08 12/22/83 MUT 7.21 25.8 < 0.005 0.817 100 < 0.05 0.164 0.078 0.012 < 0.050 12/28/83 EFF

< 0.050 0.822 103 < 0.05 0.205 0.094 7.84 12/28/83 MUT 0.82 82 < 0.05 0.183 0.067* 0.006 < 0.050 1/11/84 EFF 0.83 82 < 0.05 0.177 0.0564 8.60 < 0.050 1/11/84 MUT

< 0.005 0.82 87 < 0.05 0.105 0.062* 7.96 < 0.050 1/12/84 MUT 6.80 26.5 0.85 93 < 0.05 0.066 0.077* 0.007 < 0.050 1/26/84 EFF 0.83 87 < 0.05 0.074 0.104* 7.85 < 0.050 1/26/84 MUT

< 0.005 0.78 84 < 0.05 0.155 0.104* 8.62 < 0.050 1/30/84 MUT 7.03 26.6 0.78 82 < 0.05 0.135 0.109* 0.008 < 0.050 2/8/84 EFF 0.75 93 < 0.05 0.138 0.029* 8.83 < 0.050 2/8/84 MUT 25.7 < 0.005 0.82 86 < 0.05 0.183 0.139* 7.79 < 0.050 2/16/84 MUT 6.81 .

• Concentrator Column Analysis

Table 6-16 Analytical Data for Test 2-6th Operating Cycle

' CON D . ' H 24 S0 23 DATE p mho D.O. Li B F C1 4 TAKEN SOURCE pH 1 cm (PPM) (PPM) (PPM) (PPM) (PEM) (PPM) (PPM) (PPM)

TARGET MUT 5.0 < 0.010 0.7 90 0.05 0.05 o,05 2.6 CHEMISTRY LEVELS to to to to to to to 7.5 1.0 110 0.15 0.15 0.15 10

< 0.05 0.325 0.164 < 0.05 < o.05 6.83 24.7 < 0.005 0.82 98 3/13/84 MUT 0.87 104 < 0.05 0.448 0.170 0.06 < 0.05 3/14/84 EFF 0.82 108 < 0.05 0.388 0.179 < 0.05 < 0.05 3/14/84 MUT

< 0.005 0.80 103 < 0.05 0.388 0.297 5.05 < 0.05 3/21/84 MUT 7.09 24.9 0.83 100 < 0.05 0.331 0.109 < 0.05 < 0.05 3/28/84 EFF 0.81 88 < 0.05 0.311 0.152 3.96 < 0.05 3/28/84 MUT 25.1 < 0.005 0.81 91 < 0.05 0.308 0.150 4.83 < 0.05 4/5/84 MUT 7.05 0.83 98 < 0.05 0.323 0.127 0.23 < 0.05 4/12/84 EFF 0.81 97 < 0.05 0.307 0.154 6.95 < 0.05 4/12/84 MUT 7.18 25.3 < 0.005 0.83 98 < 0.05 0.320 0.122 6.96 < 0.05 4/19/84 MUT 0.84 99 < 0.05 0.359 0.095 < 0.05 < 0.05 4/25/84 EFF .

0.83 99 < 0.05 0.347 0.129 6.77 < 0.05 4/25/84 MUT 7.30 25.3 < 0.005 0.82 101 < 0.05 0.243 0.169* 2.0 < 0.05 5/9/84 MUT

• Concentrator Column Analysis

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

i Table 6-17 ANALYTICAL CHEMISTRY RESULTS FOR LOOP 3 DURING CLEANUP AND PRECONDITIONING Sample S0 2-B Li Date Source (PPM) (PPM) (PPM) Remarks 2/3/83 EFF 2.950 -- --

Final Water Flush 2/4/83 MUT 0.148 -- --

Preconditioning 2/4/83 EFF 1.200 -- --

Preconditioning 1

2/7/83 MUT 0.150 -- --

Preconditioning 2/7/83 EFF 0.154 -- --

Preconditioning 2/8/83 MUT 0.150 -- --

Preconditioning 2/8/83 EFF 0.152 -- --

Preconditioning 2/9/83* MUT 0.142 2389 2.04 Preconditioning 2/9/83* EFF 0.154 2296 1.92 Preconditioning Analysis performed at Waltz Mill; others done at Westinghouse Research and Development Center 65

I-I i

Table 6-18 ANALYTICAL CHEMISTRY RESULTS FOR LOOP 4 DURING ]

CLEANUP AND PRECONDITIONING Sample S0[' B Li Date Source (PPM) (PPM) (PPM ) Remarks l

2/8/83 MUT 0.007 -- --

H2 O Flush l 2/9/83 EFF 0.225 -- --

Final Flush Sample 2/10/83 MUT 0.147 -- --

Preconditioning 2/10/83 EFF 0.810 -- --

Preconditioning

]

'2/11/83 MUT 0.152 -- --

Preconditioning 2/11/83 EFF 0.373 -- --

Preconditioning 2/14/83 MUT 0.155 -- -- Preconditioning

] 2/14/83 EFF 0.183 -- --

Preconditioning

! 2/15/83 MUT 0.150 -- --

Preconditioning i

j 2/15/83 EFF 0.340 -- --

Preconditioning l 2/16/83 MUT 0.150 -- --

Preconditioning i 2/16/83 EFF 0.175 -- --

Preconditioning l

l *2/17/83 MUT 0.135 2385 2.11 Preconditioning .

1 I *2/17/83 EFF 0.147 2294 2.57 Preconditioning I i

• Analysis performed at Waltz Mill; others done at Westinghouse R+D.

t i

i 4

k

, r 1

l I

t j 6-43 4

1

,--w_ - - , , -,ww-- ,-----c a---.mm-,- --%, . - - - ,--e%.- ---v - -_----.r-, .e---.4.---mv.,%----y--,=--,----y v----- -

i Table 6-19

, APPARATUS CHANGES AND EVENTS: PEROXIDE CLEANING RUNS i

Date Event Action Result 1

2/22/83 No mixing of chemical Attached peristaltic Better solution additions in MUT pump to MUT to func- homogeneity tion as a mixing loop 1

j 2/24/83 Hourly H202 Added automatic Steady addition

}

addition H02 2 injector of peroxide to to system the system (5 al/h initially)

) 2/25/83 Plastic line on Replaced line 8 L of solution peristaltic pump lost before broke repair 2/25/83 Rupture disk broke. Replaced disk, 19 L of solution l Solution pumped to replumbed so that lost before j drain. in event of a future repair rupture the solution would be returned to the NUT l 2/26/83 Line on peristaltic Replaced line and 8 L of solution pump failed again peristaltic pump lost before with a centrifugal repair rotary pump 2/26/83 Low MUT Level Added 50 L of 54.85 L in MUT

{ solution l

2/28/83 Low flow (1.8 sph) Checked and replaced No disk rupture; l through samples rupture disk possible leakage 1 '

3/16/83 AC pressure gauge None Possibility there

broken on auto- was a bulk AC l

clave 4 pressure through the entire test period 4

i P

6-44 t

Table 6-20 AVERAGE DAILY MAKE-UP TANK PEROXIDE CONCENTRATIONS AND pH VALUES Average H,02 Concentration Date (ppm) Average pH l 2/22/83 15.0 0 (5)* 8.233 1 0.004 (3)*

2/23/83 14.9 t 2.3 (28) 8.219 1 0.008 (24) l 2/24/83 17.8 3.4 (28) 8.211 1 0.012 (9) l 2/25/83 17.9 1 3.3 (24) 8.243 (1) 2/26/83 15.6 1 2.2 (24) 8.240 0.0 (2) 2/27/83 16.5 t 1.2 (22) 8.230 ! 0.010 (2) 2/28/83 17.2 1 1.9 (24) 8.195 1 0.045 (2) 3/01/83 17.8 1 1.4 (24) 8.190 1 0.020 (2) 3/02/83 18.2 1 1.4 (24) 8.195 t 0.035 (2) 3/03/83 18.5 t 1.6 (24) 8.190 1 0.030 (2) 3/04/83 18.7 1 0.7 (24) 8.180 1 0.010 (2) 3/05/83 18.4 1 0.7 (24) 8.170 1 0.020 (2) 3/06/83 18.5 0.8 (24) 8.210 1 0.000 (2) 3/07/83 17.6 1 0.6 (24) 8.200 ! 0.000 (2) 3/08/83 17.5 t 1.4 (24) 8.180 1 0.020 (2) 3/09/83 18.3 1 1.1 (24) 8.195 t 0.005 (2) 3/10/83 17.4 1 1.1 (24) 8.175 1 0.005 (2) 3/11/83 17.6 1 1.4 (24) 8.190 1 0.030 (2) 3/12/83 19.4 1 1.0 (24) 8.16 (1) 3/13/83 18.4 1 1.3 (24) 8.180 t 0.020 (2) 3/14/83 18.7 0.9 (24) 8.150 1 0.000 (2) 3/15/83 18.3 1 0.9 (17) 8.160 1 0.010 (2)

(up to shutdown initiation)

• The number in ( ) is the number of readings over which the average is taken. The peroxide concentrations were generally determined hourly (approximately), and the pH was usually read twice daily.

6

__-45

i Table 6-21 DAILY PEROXIDE USAGE (50,000 ppe H 022 Solution)

Total Weight Average Weight Total H 0 2/ Day H0 Date Hours al Used 2(g) 2 (2 Per Hour ag/h) l 2/22/83 3.55 27.2 1.360 383 2/23/83 24 135 6.750 281 2/24/83 24 198.3 9.915 413 2/25/93 24 120 6.000 250 2/26/83 24 192 9.600 400 2/27/83 24 192 9.600 400 2/28/83 24 192 9.600 400 3/01/93 24 202 10.100 421 3/02/83 24 192 9.600 400 3/03/83 24 191 9.550 398 3/04/83 24 192 9.600 400 3/05/83 24 192 9.600 400 3/06/83 24 192 9.600 400 3/07/83 24 192 9.600 400 3/08/83 24 178 8.900 371 3/09/83 24 165 8.250 344 l 3/10/83 24 175 8.750 . 365 3/11/83 24 179 8.950 373 may be lower than reported 3/12/83 24 154 7.700 321 3/13/83 24 154 7.700 321 3/14/83 24 - 143 7.150 298 3/15/83 16 101 5.050 316 l

6-46

. . _ . _ _ _ . _ ___ _ _ _ _ _ _ _ _ _ _ . _ . _ _ . __ __._.._m _ _ _ .-. _ m

__-m . . _ _ . ._ . _ - .. . _ _ . -.

I Table 6-22 PEROXIDE LOOP ANALYTICAL DATA CLSMJIATIVE SO4 2 B LI TIME 24 SAMPLE RDMRKS i

SOURCE RLNNING 110URS (PMI) (PMO (ppb 8 DATE IGR CIDCK 0.052 2534 2.05 No Recirculation

• 02/18/83 Miff

0.273 2573. 2.14 System Flush 1400 EFF 02/18/83 2.29 From AC Bleed Line j

AC EFF 0.400 2581 02/22/83 1850 0.863 2579 2.44 Initial Sol'n. 'Ihrough -

02/22/83 1900 EFF Start W ns 2010 --- 00.00 --- --

02/22/83 13:22 0.284 2579 2.53 0932 EFF

02/23/83 EFF 16

20 0.305 2590 2.58 02/23/83 1230 37:22 0.344 2584 2.54 l

[

02/24/83 0930 1130 EFF EFF (3:20 0.388 2648 1.67 .

02/25/83 EFF 71:50 0.388 2542 1.59 02/25/83 2100 4

Mir 87:00 0.209 2407 1.59

. 02/26/83 1110 2100 EFF- 120:50 0.243 2423 1.54 02/27/83 EFF 134:35 0.226 2420 1.56 02/28/83 1045 EFF 145.50 0.263 2392 1.85 02/28/83 2200 EFF 158:50 0.263 2373 1.88 l 03/01/83 1100 EFF 167:50 0.305 2386 1.86 03/01/83 2000.

EFF 183:00 0.243 2387 1.54 03/02/83 1110 EFF 191:50 0.300 2375 1.89 03/02/83 2000 j -

EFF 209:30 0.305 2390 1.86.

I 03/03/83 1330 2000 EFF- 215:50 0.320 2368 1.87 03/03/83 EFF 233.30 0.308 2351 1.94 03/04/83 1340 EFF 239.50 0.313 2375 1.87 03/04/83 2000 i

t l

l

~

i Table 6-22 (Continued)

W F,2, CIMJIATIVE 4 B Li TDE 24 SOURCE rut #31NG HOURS (PIN) (PPM) (PIN)

DAE HOUR CIDCX EFF 253:50 0.316 2370 1.88 3/5/83 1003 3/5/83 2000 EFF 263:50 0.305 2351 1.85 3/6/83 1100 EFF 278:50 0,311 2370 1.97 3/6/83 2100 EFF 288:50 0.313 2362 1.82 3/7/83 1103 EFF 303:00 0.315 2364 1.91 3/7/83 2200 EFF 313:50 0.306 2311 1.81 3/8/83 2100 EFF 336:50 0.290 2313 1.79 3/9/83 1115 EFF 351:05 0.293 2331 1.79 3/9/83 2300 EFF 361:50 0.322 2331 1.78 3/10/83 1130 EFF 375:20 0.286 2335 1.74 3/10/83 2000 EFF 383:50 0.318 2302 1.80 3/11/83 1115 EFF 399:05 0.354 2322 1.76 -

3/11/83 2200 EFF 409:50 0.340 2318 1.82 3/12/83 1100 EFF 422:50 0.325 2285 1.78 ,

3/12/83 2300 EFF 434:50 0.345 2289 1.79 3/13/83 1115 EFF 447:05 0.325 2287 1.86 l 3/13/83 2300 EFF 458:50 0.332 2296 1.86 l

3/14/83 1105 EFF 470:55 0.309 2280 1.77 3/14/83 2300 EFF 482.50 0.317 2269 1.79 t

Table 6-22 (Continued) 4 B Li TIME 24 SAMPLE CINULATIVE (PPM) (PPM) (PPM)

HOUR CLOCK SOURCE RUttlING HOURS DATE EFF 495:05 0.324 2285 1.84 3/15/83 1115 EFF 499:50 0.331 2285 1.80 3/15/83 1600 MLfr 503:20 0.327 2287 1.79

. 3/15/83 1930 MLrr 515:50 0.365 2289 1.71 3/16/83 0800 EFF 515:50 0.370 2267 1.68 3/16/83 0800 EFF 527:20 0.348 2236' 1.72 3/16/83 1930 i

S EFF .= Imp Effluent MJr = Make-Up Tank 4

1 0

l l

l Table 6-23 Analytical Data for Test 3-HFT Cycle

,COND , SO NH S0 DATE p sho D.O. Li B F C1 4 24 23 TAKEN SOURCE pH cm ' (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) ~(PPM) (PPM)

TARGET MUT 5.0 <0.010 2.2 2300 0.05 0.05 0.05 2 CHEMISTRY LEVELS to to to to to to to --

7.5 2.5 2400 0.15 0.15 0.15 10 5/9/83 before start 1.88 2357 <0.010 0.319 0.118 11.95 <0.05 5/25/83 MUT 1.92 2371 <0.G5 0.305 0.128 3.95 <0.05 5/25/83 EFF 1.94 2360 <0.05 0.455 0.244 0.09 <0.05 6/3/83 MUT 5.52 47.8 SAT 1.98 2339 <0.05 0.301 0.103 5.82 <0.05 6/8/83 MUT 1.98 2334 <0.05 0.273 0.143 1.99 <0.05 6/8/83 EFF 1.98 2337 <0.05 0.282 0.136 0.41 <0.05

k f

Table 6 Analytical Data for Test 3-Ist Operating Cycle SO NH S0 COND C1 4 24 23 3

B' F

'p mho D.O. Li (PPM) (PPM) (PPM)

DATE (PPM) (PPM) (PPM)

SOURCE pH cm J (PPM) (PPM) 2 TAKEN 2.2 1180 0.05 0.05 0.05 2 5.0 <0.010 to to --

TARGET MUT to to to to CHEMISTRY LEVELS to 2.5 1220 0.15 0.15 0.15 10 7.5 1175 <0.05 0.223 0.117 8.98 6.07 43.7 0.005 2.06 6/27/83 HUT 1192 <0.05 0.264 0.116 8.83 2.08 6/29/83 MUT 0.231 0.122 <0.02 2.08 1182 <0.05 6/29/83 EFF

<0.05 0.394 0.127 8.8 <0.05

<0.005 1.96 1028 7/12/81 MUT 6.13 44.8 '

1090 < 0'. 0 5 0.419 0.130 9.1 <0.05 MUT 1.92 7/13/83 0.164 <0.01 <0.05 2.22 1196 <0.05 0.406 7/13/83 EFF 1041 <0.05 0.377 0.122 9.64- <0.05 MUT 1.83 7/27/83 0.62 <0.05 1.79 1105 <0.05 0.437 0.120 7/27/83 EFF 0.93 1190 <0.05 0.232 0.108 9.69 "QNS"*

6.06 46 <0.005 8/1/83 MUT 9.17

'2.08 1206 <0.05 0.230 0.111 "QNS" 8/10/83 MUT 0.17 2.02 1183 <0.05 0.235 0.115 "QNS" 8/10/83 EFF 1233 <0.050 0.239 0.107 7.36 <0.05 MUT 6.11 44.3 0.005 2.04 8/22/83 8.48 <0.05 2.03 1127 <0.050 0.247 0.113

> 8/24/83 MUT 0.018 <0.05 2.04 1152 <0.050 0.253 0.113 8/24/83 EFF

• Quantity not sufficient for analysis

. ^ - - . - - _ _

i Table 6-25 Analytical Data for Test 3--2nd Operating Cycle SO NH S0 23

,COND F C1 4 24 p mho' D.O. Li B DATE (PPM) (PPM) (PPM) (PPM)__

(PPM) (PPM) (PPM)

SOURCE pH cm '

(PPM) .

TAKEN 1.7 980 0.05 0.05 0.05 2 TARGET MUT 5.0 <0.010 to to --

to to to to CHEMISTRY LEVELS to 0.15 0.15 0.15 10 7.5 2.0 1020 967 <0.05 0.224 0.126 8.75 MUT 6.23 40.7 0.005 1.41 9/16/83 0.113 8.97 1.36 982 <0.05 0.227 9/21/83 MUT Q.245 <0.01 1.40 976 <0.05 0.235 9/21/83 EFF 1.45 957 <0.05 0.224 0.137 9.34 6.13 40.0 <0.005 9/30/83 MUT 0.133 8.52 1.45 986 <0.05 0.217 10/5/83 MUT

<0.01 1.52 978 <0.05 0.235 0.121 10/5/83 EFF 1.45 976 <0.05 0.237 0.121 9.78 10/19/83 MUT 1.47 980 <0.05 0.233 0.134 3.92 10/19/83 EFF 1.46 978 <0.05 0.230 0.120 9.78 MUT 6.07 40.2 <0.005 10/20/83 1.64 1007 <0.05 0.152 0.121 9.64 11/2/83 ' MUT 1.64 1009 <0.05 0.151 0.152 0.027 11/2/83 EFF

<0.05

<0.005 1.63 982 <0.05 0.412 0.073 8.76 11/8/83 MUT 6.04 39.3 1.70 9 86 <0.05 0.328 0.103 0.012 <0.05 11/16/83 EFF 1.58 989 <0.05 0.408 0.074 9.46 <0.05 11/16/83 MUT

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

Table 6-26 Analytical Data for Test 4-!!FT Cycle S0 N2 "4 23 B- F Cl 4 DATE t a o' D.O. Li (PPM) (PPM) (PPM)..

(PPM) (PPM) (PPM) (PPM)

TAKEN SOURCE pH cm i (PPM)

<0.010 2.2 2300 0.05 0.05 0.05 2 TARGET MUT 5.0 to to to --

to to to CHEMISTRY LEVELS to 2.5 2400 0.15 .0.15 0.15 10 7.5 1.93 2401 <0.01 0.319 0.118 0.08 <0.05 5.55 45.6 <0.005 5/19/83 MUT 4.34 <0.05 1.99 2339 <0.05 0.307 0.118

? 5/25/83 MUT 1.95 2382 <0.05 1.070 .0.408 0.02 <0.05 5/25/83 EFF 1.90 2334 <0.05 0.317 0.336 3.10 <0.05 6/3/83 HUT 5.46 44.4 SAT 1.96 2338 <0.05 0.293 0.337 1.81 <0.05 6/8/83 EFF 1.97 2341 <0.05 0.307 0.314 3.18 <0.05 6/8/83 MUT P

~ - - _ - - _ _ _ _ _ _ _

Table 6-27 Analytical Data for Test 4 -Ist Operating Cycle 0

F C1 4 2"4 23 o' D.O. Li B DATE (PPM) (PPM) (PPM) (PPM) pH cm (PPM) (PPM) (PPM) (PPM)

TAKEN SOURCE

<0.010 2.2 1180 0.05 0.05 0.05 2 TARGET MUT 5.0 to to to --

to to to CHEMISTRY LEVELS to 0.15 10 2.5 1220 0.15 0.15 7.5

<0.05 0.213 0.117 8.24 <0.05 6.04 44.0 <0.005 2.07 1199 6/27/83 MUT

<0.05 2.01 1199 <0.05 0.213 0.110 9.09 6/29/83 MUT

<0.05 2.04 1171 <0.05 0.246 0.136 <0.02 6/29/83 EFF

<0.05

<0.005 1.95 1138 <0.05 0.396 0.126 9.0 7/12/83 MUT 6.11 54.4

[ 1198 <0.05 0.390 0.120 7.3 <0.05 1.89 7/13/83 MUT 1.93 1191 <0.05 0.558 0.357 <0.01 <0.05 7/13/83 EFF

<0.05 1.91 1170 <0.05 0.457 0.122 0.08 7/27/83 MUT 1.86 1155 <0.05 0.455 0.127 <0.02 <0.05 7/27/83 EFF 2.12 1206 <0.05 0.260 0.131 8.64 <0.05 8/2/83 MUT 6.06 45.0 0.005 2.05 1159 <0.05 0.239 0.115 8.72 "QNS"*

8/10/83 MUT 2.04 1165 <0.05 0.242 0.115 0.004 "QNS" 8/10/83 EFF 0.005 2.03 1167 <0.05 0.250 0.114 8.36 <0.05 8/22/83 MUT 6.08 44.1 2.06 1180 <0.05 0.244 0.113 8.84 <0.05 8/24/83 MUT 2.06 1178 <0.05 0.258 0.113 0.004 <0.05 8/24/83 EFF

• Quantity not sufficient for analysis

4 J-Table 6-28 Analytical Data for Test 4-2nd Operating Cycle 0 NH S

'p m o' D.O. Li- B F Cl 4 y4 23 DATE TAKEN SOURCE pli cm n (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) l TARGET MUT 5.0 <0.010 1.7 980 0.05 0.05 0.05 2 to to to to to to --

CHEMISTRY LEVELS to 7.5 2.0 1020 0.15 0.15 0.15- 10 6.13 38.8 <0.005 1.43 967 <0.05 0.230 0.235 <0.01 p 9/16/83 MUT

$ 1.36 927 <0.05 0.232 0.216 0.03 9/21/83' MUT i

1.39 927 <0.05 0.239- 0.295 <0.01 9/21/83 EFF 9/30/83 MUT 6.20 40.4 <0.005 1.42 927 <0.05 0.234 0.139 6.7) i 10/5/83 MUT 1.51 980 <0.05 0.232 0.149 9.15 10/5/83 EFF 1.46 978 <0.05 0.233 -0.146 <0.01 10/19/83 MUT 1.54 980 <0.05 0.246 0.143 9.22 10/19/83 EFF 1.48 978 <0.05 0.250 0.146 3.92 10/24/83 MUT 6.03 40.2 <0.005 1.65 1010 <0.05 0.151 0.127 6.86 11/2/83 MUT 1.65 1011 <0.05 0.160 0.126 8.11 11/2/83 EFF 1.65 1005 <0.05 0.170 0.122 0.025 11/15/83 MUT 6.23 40.2 <0.005 1.60 1004 <0.05 0.416 0.078 9.62 <0.05 11/16/83 EFF 1.53 992 <0.05 0.214 0.132 0.009 <0.05 11/16/83 MUT 1.64 994 <0.05 0.186 0.080 10.28 <0.05

1 Table 6-29 Analytical Data for Test 3-3rd Operating Cycle DATE 'u l o' D.O. Li B F C1 4 2"4 23 TAKEN SOURCE pH cm I (PPM) (PPM) (PPM) (PPH) (PPH) (PPM) (PPM) (PPH)

TARGET MUT 5.0 <0.010 1.0 490 0.05 0.05 0.05 2.0 CilD!ISTRY LEVELS to to to to to to to 7.5 1.3 510 0.15 0.15 0.15 10 12/13/83 MUT 6.4 34.2 <0.005 1.048 495 <0.05 0.374 0.224 9.53 <0.050 12/15/83 EFF 1.034 495 <0.05 0.224 0.098 0.035 <0.050 12/15/83 MUT 1.064 496 <0.05 0.280 0.141 9.66 <0.050 12/22/83 MUT 6.41 33.3 <0.005 1.047 495 <0.05 0.322 0.180 9.19 <0.050

{

12/28/83 EFF 1.062 487 <0.05 0.375 0.070 0.026 <0.050 12/28/83 MUT 1.049 495 <0.05 0.291 0.115 9.51 <0.050 1/9/84 MUT 6.28 33.3 <0.005 1.02 491 <0.05 0.310 0.087 9.22 <0.050 1/11/84 EFF 1.01 493 <0.05 0.276 0.110 0.005 <0.050 1/11/84 MUT 1.01 489 <0.05 0.195 0.094 8.93 <0.050 1/26/84 EFF 0.99 492 <0.05 0.253 0.103 0.005 <0.050 1/26/84 MUT 0.96 485 <0.05 0.285 0.073 9.20 <0.050 1/31/84 MUT 6.23 33.5 <0.005 0.96 498 <0.05 0.289 0.079 9.17 <0.050 2/8/84 EFF 1.02 492 <0.05 0.271 0.099 0.008 <0.050 2/8/84 MUT 0.98- 501 <0.05 0.237 0.093 8.21 <0.050 2/14/84 MUT 6.54 33.6 <0.005 1.00 492 <0.05 0.290 0.085 9.17 <0.050

- Teble 6-30 Analytical Data for Test 3-4th Operating Cycle

,COND , SO N II S6 DATE p mho '

D.O. Li B F Cl- 4 24 23 .

TAKEN SOURCE pil cm (PPM) (PPM) (PPM) '( P PM ) ' (PPM) (PPM) (PPM) (PP!')

TARGET }R'T 5.0 < 0.010 0.7 90 0.05 0.05 0.05 2.0 CilEMISTRY LEVELS to to to. to to to to 7.5 1.0 110 0.15 0.15 0.15 10 .

.3/13/84 MUT '6.88 25.0 <0.005 0.78 97 <0.05 0.355 0.183- 2.65 <0.05 3/14/84 EFF O'.80 103 <0.05 'O.346' O.129 <0.05 <0.05-3/14/84 MUT 7.10 25.5 <0.005 0.80 101 <0.05 0.355 0.178 ,3.37' <0'.05p

^~

-3/28/84 EFF 0.81 97 <0.05 0.341 0.144' <0.05 ' <0.05 "

3/28/84 MUT

y 0.80 -101' <0.05 0.307 0,141 4.15 <0.05 4/Y/84' '5DT1 ,

7,11 25.1 <0.005 0.79 97 ,<6.05 0.303 0.155 5.62 <0,.05

+ ,

'4/12/8fi' , EFF y 0.80 99 <0.0$ 0.300 ,'.0.153 <0.05 0.090 4/12/d4 . ; rfUT ' -

0.79 101 <0.05 0.302 0.122 6.24 <0.05 4/25/84e, EFF1 ,

0.80 100 s <0.05 0.291" 0,.102 <0.05 <0.05 y 4/25/84 'MUT 6.99 24.4 . <0.005 0.80 s d59

<0.05

+c 0.329 0.135 6.37

'<0.05 -

5/10/84 EFF ,

0.86 101 <0.05 ' O.195 0.108 <0.03 <q.05 5/10/84- MUT 0.80 102 <0.05 ,0.197 0.146 3.4' . t <0. 0'5 - '

- ".- 5/14/84 MUT 7.11 ' 25.0 <0.005 0.80 99 ' ,<0.05 0.179' O.147 3.8 <0.05

+ x i '"

• 2 .

_; Concentrator Colux .Analysia O' , '..$

I e si V.

jm -%

.j

[/ s , i 3.. -

..j ' / s A

Table 6-31 Analytica1' Data for Test 4-3rd Operating Cycle

, DATE nho' D.O. Li B F C1 4 2"4 '23 TAKEN SOURCE ;H cm (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) (PPM)

TARGET MUT 5.0 <0.010 1.0 490 0.05 0.05 0.05 2.0 CilEHISTRY LEVELS :0 to to to to to to

~.5 1.3 510 0.15 0.15 0.15 10 12/13/83 MUT 6.42 33.9 .0.005 1.070 490 <0.05 0.405 0.226 6.86 <0.050 12/15/83 EFF 1.026 493 <0.05 0.258 0.098 0.017 <0.050 12/15/83 MUT 1.047 493 <0.05 0.309 0.141 7.09 <0.050 12/27/83 MUT 6.60 35.1 <0.005 1.066 506 <0.05 0.300 0.097 8.90 <0.050

{*

12/28/83 12/28/83 EFF 1.064 1.073 496 <0.05

<0.05 0.427 0.403 0.063 0.016 <0.050 MUT 500 0.050 9.49 <0.050 1/11/84 EFF 1.07 498 <0.05 0.276 0.104 0.006 <0.050 1/11/84 MUT 1.04 501 <0.05 0.299 0.060 8.95 <0.050 1/17/84~ MUT 6.52 32.7 <0.005 1.01 494 <0.05 0.248 0.100 7.91 <0.050 1/26/84 EFF 1.02 496 <0.05 0.253 0.088 0.005 <0.050 1/26/84 MUT 1.02 498 <0.05 0.299 0.079 9.17 <0.050 2/3/84 MUT 6.25 33.7 <0.005 1.03 494 <0.05 0.250 0.113 9.40 <0.050 2/8/84 EFF 1.06 498 <0.05 0.273 0.038 0.006 <0.050 1

2/8/84 MUT 1.02 496 <0.05 0.254 0.100 9.32 <0.050 4

. Table 6-32 Analytical Data for. Test 4-4th Operating Cycle j

,COND , SO . NH S0 DATE p mho . J. O. Li B F C1 4 24 23 TAKEN SOURCE pH ,

em (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) (PPM) ~(PPM)

TARGET MUT 5.0 <0.010 0. 7 ' 90 0.05 0.05 0.05 2.0  ;

CHD!!STRY LEVELS to to to to to' _ to to l 7.5 1.0 110 0.15 .0.15' O.15 10

-3/13/84 MUT 6.83 24.7 <0.005 0.81 98 <0.05 0.347 0.167 2.58 <0.05 3/14/84' EFF 0.83 99 <0.05 0.379 0.157 0.06 <0.05 )

3/14/84 MUT 7.09 24.9 <0.005 0.81 98 <0.05 0.349 0.166 2.30 <0.05 3/28/84 EFF 0.83 97 <0.05- 0.316 0.106 <0.05 <0.05 3/28/84 MUT 7.05 25.1 <0.005 0.82 97 <0.05 0.305 0.130 3.65 <0.05 I 4/9/84' MUT 0.84 98 <0.05 0.303 0.135 4.86 <0.05 4/12/84 EFF 0.84 99 <0.05 0.329 0.148 0.86 <0.05 4/12/84 MUT 7.18 25.3 <0.005 0.83 98 <0.05 0.307 0.121 5.17 <0.05 4/25/84. EFF 0.83 100 <0.05 0.349 0.106 <0.05 <0.05 4/25/84' MUT <0.005 0.83 98 <0.05 0.334 0.139 3.57 <0.05 5/10/84 'EFF 0.88 102 <0.05 0.222 0.111 <0.03 <0.05 5/10/84 MUT' O.77 100 <0.05 0.195 0.143 1.4 <0.05 5/10/84 MUT. 6'.97 .25.5' 4.005 0.80 100 <0.05 0.200 0.150 3.7 <0.05 Concentrator Column Analysis

l l

l l

I Section 7 f

d' RESULTS 1

At the end of each cycle, the specimens were removed and the

, C-rings were stereomicroscopically examined under low and high magnification. Full size tubes were then eddy current examined while j one C-ring was terminated, weighedJ and metallographically examined.

Occasionally additional examination techniques such as SEM or ESCA were employed. The remaining C-rings which completed the final cycles, (Cycle 6 for Test 1 and 2, or Cycle 4. for Test' 3 and 4), underwent exhaustive examinations as described in Section 7.4.

7.1 Visual Examination (low magnification)

Figures 7-1 through 7-23 show before and after photomacrographs l of the specimens removed from the experiments for metallographic

analysis at the end of their defined test period (see Table 6-2). The

] view is looking through the C-ring cutout slot at the stressed ID j surface. Post-test results are shown in Section 7.4. Both the inside (ID) surfaces and the outside (OD) surfaces were examined, but the l centers of the ID surfaces of the C-rings were difficult to view effectively due to the stressing bolt.

4 Interpretation of the observations is difficult since most of

! the tubes had significant surface abnormalities in the as-received condition. The primary observation following the peroxide exposure was that the material in the ID pits, which pits are typical of the ID surfaces of the as-received OTSG tubing samples, exhibited a discoloration with respect to adjacent ID surface films. This usually

^

darker discoloration differentiated the pits from the adjacent surface

!- regions to an extent that the pits appeared anomalous. However, the l number of pits, the randomness of distribution of the pits, and the a

sizes of the pits were typical of other C-ring samples which were not i

i 7-1

. . . ~ . . . .

exposed to the peroxide clean-up chemistry. Since later examinations of these peroxide pre-exposed samples following subseq2ent exposure to i

normal reactor coolant chemistry and temperatures gave observstions which were typical of all other samples, the anomalous appearance of the material 11n the pits following the peroxide run is potentially interpretable in terms of differences in the reactivity or response

~

i

- of the deposits as governed by solution accessibility and/or localized variations in the deposit topology. Following the addition of special f U-bends of core materials in the hydrogen peroxide clean-up test, all J

4 U-bends were also examined by the stercomicroscopy technique af ter each individual run in simulated reactor coolant. These examinations showed no surface abnormalities. The peroxide exposure therefore, had no visually detrimental effects on the materials. Retrospectively, none of the examinations revealed any serious corrosion effects such as ID-initiated cracking or pit propagation.

' Most of the specimens that went through the long term corrosion j test cycles had significant mechanical markings (scratches and score marks) and pitting. However, these were generally associated with 3

the "as-received" surface features.

1 7.2 Weight Changes I

I Weight changes of C-rings removed from test during the course

! of the experiments are shown in Table 7-1. The average' change was a j

0.03 percent weight loss. Table 7-1 also shows the dates and cycles, when the specimens were removed.

' 7.3 Meta 11ographic Examination (high magnification)

A metallographic examination was made of each C-ring removed from the test af ter their defined cycle. Post test results are shown j

in Section 7.4. Each specimen was transversely sectioned. One midplane and one end surface were mounted and polished. Etched surfaces were -

l prepared by a 60 second exposure to concentrated HC1, methanol rinse, 5-10 second exposure to 2 percent-bromine in methanol, and two 4

additional methanol rinses.

]

4 7-2

t 5-i 1

{: Typical micrographs of the stressed region, ID surfaces of each e

1 specimen, are shown in Figures 7-24 through 7-58. No unusual surface features were observed in any of the specimens except 1B4. Surfaces examined have shown intergranular attack to a maximum depth of one to two' grains. For C-ring 1B4 removed after cycle 5 (during this last

. reporting period),. three areas of further intergranular attack were

found. These were all in the I.D. surface and occurred in the end

] metallographic plane. Micrographs of three areas are shown in Figures 7-59 through 7-61. The depth of, attack varied from 0.002 inches to 0.010 inches. Figure 7-62 shows the location of the three areas of i

attack in the cross-section of the C-ring.

The " midplane" metallographic section of 1B4 was removed from the mount and remounted and polished after an additional 0.05 inch

] depth removal. One. additional area of attack, located about 45 4

degrees between the stressed region and the bolt hole,'was found j (Figure 7-62).

~

l The "end" metallographic section of IB4 was fiatiened and examined.

j for " opened" defects. A photograph of the flattened I.D. surface is shown in Figure 7-63. Several cracks and pits were found. The results from these metallographic examinations are discussed in Section 8.2. '

7.4 Post-Test Metallographic Examination 7.4.1 Experimental Procedures I

C-ring Specimens 4

~

The procedure used for the C-ring analyses was as follows:

, 1. Each specimen was visually examined and weighed..

i j 2. Specimens were bent to achieve 3% additional l plastic surface strain.

- *3. Each specimen was visually re-examined.

} 4. Representative specimens were selected for

, optical metallography using a 1/4" ring.

Remainder was used in Step 5.

M l.

1 i

. . 7-3

_ . _ . - , , , . . - , . , w - , .+., - . . , . . . , . , - . - - - . , ,,.n... - - ,_

• 5. Specimens were flattened and visually re-examined.

• 6. Each specimen was stressed to yield a 90* reverse bend, and visually re-examined.

At each step indicated by an *, any new defects observed were reported to GPU before proceeding further.

U-Bend Specimens All U-bend specimens and the Zircaloy C-ring specimens were l subjected to the same evaluation sequence:

1. Each specimen was visually examined.

2. Specimen 1 cgs were squeezed together to achieve the TLTA condition and specimens were then visually re-examined.

3. Metallography was performed on one specimen of each material.

Full Tube Specimens The general scheme for examination of the full tube specimens is given below. However, due to the presence of cracks in some tubes, more specific procedures were utilized. Thus, a "roadmap", specific to each tube, which outlines all examinations and sectioning, is included with the results in Section 7.4.2. All hardware was removed from the tubes before visual examinations were performed. A maximum of 0.2" of tube was lost in this procedure - more generally <0.1" - at both the top and bottom.

1. Each tube 0.D. was visually examined and pencil probe eddy current analysis was performed.

2. Tubes were then split longitudinally and the I.D.'s visually examined.

A Two legs together 7-4

t 1

3. Specimens with visible cracks were sectioned to perform metallography and/or SEM/EDS evaluation.

4. Remaining tube halves were pulled in tension to N10% plastic strain.

5. Both 0.D. and I.D. of the tubes were visually examined. Selected crack regions were further examined by optical metallography and/or SEM/EDS.

, Previously unreported changes were discussed with GPU at each stage. l (All specimen sectioning was performed using a Buehler radial saw with a 0.045" blade thickness) .

Microstructural Analysis i All optical metallography was performed on standard mounted specimens using normal sic grinding procedures going from 100 to 600 grit sic and (for Inconel 600) following with a 6 um diamond polish on i white duck canvas and a finish polish (<0.05 pm) on microcloth. Specimens were etched to reveal grain boundaries using the standard bromine-etching procedure, comprised of the following:

1. Immerse in 100% hcl for 60 sec. to remove any passivation layer.

2. Rinse with methanol.

3. Etch with a 2% bromine in methanol solution for between 8-20 sec.

4. Rinse in methanol bath (repeat).

SEM/EDS investigations were performed on either a Cambridge Stereoscan S4 or 150MK2, both of which are equipped with KEVEX 7000 analytical energy dispersive X-ray spectrometers. A 20 kv accelerating-voltage was utilized. Qualitative X-ray spectra were obtained where l

l required to determine the presence of impurity species in the inter-granular cracked regions.

7-5

._____m..- _ __ ._. ~ _ _ _ _ . _ _ . . _ -

I' i

Specimen Straining i

i Full tube specimen sections were. strained to yield approximately 10% strain by loading in tension with an Instron and monitoring gage 1.

! length extension. For the C-ring-specimens, the deflection required to.

i produce an additional 3% plastic surface strain was calculated and applied to the specimen using a simple jig constructed from a' C-clamp arrangement. Flattening of the specimen incurred a maximum of 13%

5 plastic strain.

7.4.2 Results

! C-rings C-ring specimens examined were 1Al, lA4, PIAS, 1B2, 1B3, IB5, 2A1, 2A4, P2A5, 2Dl, 2D3 and the GPU archive C-rings exposed to 6 operating cycles at Westinghouse, lE2, lE3, lE6, lE4 (corresponds to l

GPU's lE7 designation). Remaining C-rings were weighed and stored,

namely 1D2,1D3, 2B1, 2B3, PlD3, P1D4, P1D5, lA3, ID6, ID7, ID8, 2AS, i 1E8A, lE7A. Table 5-2 in the 1st interim report references the C-ring l2 origin. C-ring P2D2 was removed for Auger analysis during the 3rd cycle and cut-into 3 pieces. It was not therefore used in the final

-l r 1 microstructural investigation. ._

i j

A summary of the C-ring testing and evaluation is presented in

_I Table 7.2. Figures 7 7-88 show macro-optical photographs of-the f C-rings before and after their respective test P exposures, together with representative metallographic documentation after 3% strain. The' data 4

J are organized according to autoclave chemistry. C-rings lA1, 1B2, IB4 (metallographically mounted),1B5 (one cycle only), 2A1, 2Dl, lE2 and

-lE3 were in Loop #1 with thiosulfate chemistry. C-rings lA4, IB3, 2A4,

]

j 2D3, lE4 and lE6 were in Loop #2 exposed to sulfate chemistry, and C-rings PlA4, PlA5 and P2A5 were in Loop #3 exposed to H 022 Pl us sulfate

, chemistry.

1 f

1 7-6 i

l

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

Micrographs of Loop #1 C-rings are presented in Figures 7-64 to 7-75. Visual inspection showed that lAl, 2Al, lE2 and IE3 had no defects after flattening or the 90* reverse bend. Other C-rings had very small defects visible after various stages of the test procedure.

1B2 had a small I.D. crack network, 1/32" long, visible after 3% strain.

The optical micrograph in Figure 7-67 shows a small area of pull-out and IGA approximately 5 grains deep. 1B5 showed no defects after 3%

strain but after flattening the I.D. did show small axial cracks (no change after reverse bend). Figure 7-69 shows that IGA was localized and a maximum of 4 grains deep. 2D1 showed some small cracks (maximum was 3/16" long, circumferential) only af ter the 90* reverse bend.

Optical metallography (Figure 7-73) indicated no IGA. Finally, C-ring 1B4 had a pitted area on the I.D. which showed some localized shallow cracks after 3% strain. In summary, therefore, no throughwall defects were observed.

Micrographs of Loop #2 C-rings are presented in Figures 7-76 to 7-82. No defects were observed af ter flattening or the 90' reverse bend in C-rings lAl, lE4 or lE6. For C-rings 2A4 and 2D3, some short localized axial cracks were detected on the I.D. after flattening.

After 3% strain C-ring 1B3 showed some small cracks associated with an I.D. pitted area. A similar observation was made af ter flattening.

Optical metallography, af ter 3% strain, showed an IGA region approximately 10 mils deep. This defect was the most severe detected on any of the C-rings evaluated.

Loop #3 C-ring micrographs are shown in Figures 7-83 to 7-88.

Both PlA5 and P2A5 showed no defects after either flattening or the 90' reverse bend. Optical metallography performed after 3% strain (Figures 7-86 and 7-88, respectively) revealed no evidence of IGA. PlA4 also showed no evidence of defects af ter flattening or the 90' reverse bend 7-7

on the I.D. The 0.D. had some indication of small cracks after 3% strain.

Metallography (Figure 7-84) showed some local IGA on the 1.D. which is 1-3 grains deep.

U-Bend and Zircaloy-4 C-ring Specimens Macro-opticals of the as-tested and strained specimens, together with representative metallography, are presented in Figures 7-89 to 7-102.

U-bends fabricated from 410 SS (Figure 7-96), 304 SS (Figures 7-97 and 7-98), Inconel 82 cladding on Inconel 600 (Figures 7-92 and 7-93) and 308 SS cladding on 304 SS (Figures 7-99 and 7-10@ showed no evidence of cracking, although for the latter material, Specimen D2 did show a defect with pull-out on one side of the weld bead. The Inconel X-750, (Figures 7-89 to 7-91) and 17-4 PH (Figures 7-94 and 7-95) U-bends and the Zircaloy-4 C-rings (Figures 7-101 and 7-104 all showed ductile fracture when strained to the TLT condition as part of the post-test examination. All metallography was performed at the region of highest strain. SEM analysis of the Inconel X-750 U-bend Q11 confirmed that the fracture was entirely dimpled rupture with no intergranular f racture (Figure 7-91) . The behavior of the Zircaloy-4 C-rings was compared to the behavior of a dummy specimen with no autoclave exposure and found to be very similar (Figure 7-104 Full Tube Specimens The procedure described in Section 7.4.1 applies to lead test specimens A16-69 (6 1/2" - 12 1/4"), A88-7 (2" - 9 3/4"), A13-63 (11" -

18 15/16") and A24-94 (19 5/16" - 25 7/16") and repair test specimen A24-94 (36" - 42"). Tubes B94-27 (4 1/2" - 10 1/2") and B16-22 (52" -

59") were subjected only to a visual examination before being stored.

Each tube is discussed on an individual basis to maintain clarity.

The lengths and distances reported refer to the tubes in their present condition. These dimensions do not account for the 0.2 - 0.4" lost during post-test hardware removal. Thus, an error of this order should be considered in comparing these lengths with the original values. Further 7-8

I

)

i reference to OTSG distances can be made using the original lengths re-ported in Section 7.4.1. Table 7-3 provides a summary of the full tube defect observations.

Tube A16-69 (Lead Test)

The roadmap for this tube is given in Figure 7-103. Visual 4

inspection of the 0.D. showed 3, very short, circumferential crack-like features 3/8" below the top. Thus, a ring 1/2" long was removed to preserve these ' defects before axial cutting and pulling were performed.

No eddy current indications were observed in this region.

l The pencil probe did detect a 1/2" long circumferential crack 2 1/8" from the bottom of the tube centered at approximately 90*.

Previous eddy current testing had reported this indication approximately at the middle of the tube.( } The

~

j pencil probe finding was confirmed by the visual I.D. inspection, which 1

also identified a second 5/16" long crack network N1/8" closer to the l

top of the tube. The tube was then sectioned axially such that this l

i defect was entirely contained in the 90* half, which was further sectioned, as indicated in Figure 7-103, to yield pieces 1A,1B and IC.  !

Optical metallography was performed on a cross-section of the crack in

!, piece IB (Figure 7-104) to show the extent of IGA which is throughwall.

An additional area of I.D. ICA in piece 1B is presented in Figure 7-105.

Penetration is approximately 50% of the wall thickness.

l Piece 1C from the 90* half and the entire 270* tube half were subsequently strained. No cracks were detected in the former piece af ter straining, but in the 270* half, a crack located N1" from the top i

of the tube (i.e. 1/2" from the top of the piece strained) opened. This defect, documented by macro-optical micrographs in Figure 7-106,was further analyzed by SEM (Figure 7-107 af ter breaking open the crack.

ICA appears to occur through N60% of the wall thickness'from the I.D.

over a circumferential distance of N.16".

! 7-9

Tube A88-7 (Lead Test-)

The roadmap for this tube is given in Figure 7-108. The 0.D.

visual inspection revealed no defects, but eddy current testing using a pencil probe indicated a 9/16" circumferential crack ruoning from 45' - 90' - 135' at 4 1/2" from the top of the tube. This correlates with the defect this tube was known to have when received.( The tube was split along O' - 180* to contain the crack in the 90' half.

I.D. inspection confirmed the presence of a crack network at this location, associated with a deep, circumferential1y oriented, elongated and oxidized pit. This tube half was subsequently sectioned into pieces 1A,1B (containing the defect) and 1C as shown in Figure 7-108. Pieces lA and IC were strained, upon which several small cracks opened up on the I.D., but no defects were visible on the 0.D.

The crack in piece 1B was documented in the macrophotographs presented in Figure 7-109 before being broken open. The extent of IGA is clearly visible in both the optical and SEM micrographs (Figures 7-110 and 7-11L respectively). Through-wall IGA is present over a circumferential distance of NO.175" and is 1.D. initiated. EDS analyses in area 4 showed high Cr and Ni concentrations with Mn, Fe, Cu and Zn also present. Area 3 also showed high Cr and Ni, with only Mn and Fe present in smaller amounts. Area 2 showed Ni, Cr, Fe and Mn (decreasing concentrations) and possibly a minor S concentration.

Straining the 270* half opened a zone of shallow I.D. surface cracks, with some grain loss, located between 1 5/8" and 1 7/8" from the top of the tube. They were further documented by an SEM study (Figure 7-112) The tubo exhibited a " singing noise" during pulling. Many of the cracks (circumferential) were located within dark spots. They appeared to penetrate to a maximum depth of only a few grains. Optical metallography, which attempted to document the largest defect observed (area D, Figure 7-113 was unsuccessful - the small size of this region made it impossible to locate in the mounted specimen. The microscopy did confirm that most of the cracks are less than or equal to one grain diameter deep and may have resulted from straining of shallow ICA islands.

7-10

l

~

l Tube A13-63 (Lead Test)

Full tube visual inspection of the 0.D. revealed no defects, but the pencil probe located a 1/2" circumferential crack, N3" from the top of the tube, which ran 90* - 180* - 225*. The tube was sectioned into 2 halves such that the defect was contained in the 180* half, as shown in the roadmaps for the 180* half (Figure 7-113) and O' half (Figure 7-114). Note that the pre-test eddy current data reported a defect 16" from the top of the tube. Visual I.D. inspection of the 0*

half revealed no cracks, but some pitting and yellow spots werc observed. Inspection of the 180* half I.D. showed a 1/2" long circum-ferential crack N3" from the top, corresponding to the pencil probe eddy current indication. This is documented by the macro-optical micrographs in Figure 7-115. A small, tight, axial Y-shaped crack, approximately 1/64" long and located between 2 old pits, was also j observed on the I.D. of this half. It was located 6 1/2" from the top of the specimen. Yellow spots, stains and pits were detected near the top. Examples of the latter are given in Figure 7-116.

After straining the 0* half, the upper portion of the specimens contained many short, circumferential cracks located within the yellow spots noted earlier. The yellow material had a crystalline appearance.

Examples of such cracks are shown in Figure 7-117. The specimen was then sectioned to yield pieces lA,1B and 1C (Figure 7-114)in order to perform an SEM/EDS study of some of the cracked areas. Both the intergranular nature of the crack and the presence of a flaky surface deposit are clearly evident in Figure 7-118. EDS analyses showed very high S i

concentrations in Area A1, with a lesser amount present at A2 (see Figure 7-119). Cr concentrations were also high in both areas. Evaluation of several other areas yielded similar results. Optical metallography f rom a polished cross-section of area A (Figure 7-120) revealed the ICA to be approximately 33% of the wall thickness.

7-11

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

J

]

The 180* half was sectioned into 3 pieces, following the roadmap in Figure 7-113, such that the crack described earlier was contained within piece 1B. This crack was opened and studied using both optical and scanning electron microscopy. Piece 1A was subsequently strained

< 10% uhich opened up 2 additional I.D. cracks located at 15/16" and 1 1/2" from the bottom of the tube, respectively. Both were circumferential and approximately 1/64" in length.

Macro-optical micrographs of piece 1B after fracture are presented in Figures 7-121 to 7-123. An additional I.D. crack 40.1" below the lower fracture and 1/8" in length was also opened (Figure 7-122).

] This crack was not visible on the 0.D. A large pit was located near one l end of the crack and a second, smaller pit in the center.

j The extent of IGA in the original crack is well documented by l

1 Figures 7-123 and 7-124. Through vall penetration had occurred over a circumferential distance of 40.31". The attack appears to have been I.D.

initiated. EDS analyses, performed to detect grain boundary contaminants, j i suggested the presence of S only towards I.D. edges of the ICA, for example in regions b2 and b5. However, the concentration of the element

present was insufficient to positively distinguish between S and Mo.

I Tube A24-94 (Lead Test)

Post-test pencil probe eddy current testing indicated 3 cracks in this tube specimen. These were respectively, 1) a circumferential crack 91 1/2" long (270' - 0* - 135*) located 1 5/8" from the top; 2) a circumferential crack N1" long (45' - 0* - 215') located 1/4" from the bottom; 3) a crack (almost circumferential in nature, but inclined N70*

1 with the longitudinal axis) 41/2" long (45' - 0* - 315*) located 3/4" from the bottom of the tube. This latter crack yielded no 0.D. visual indication. The other two defects were observed on the 0.D. by visual inspection. The defect located 1 5/8" from the top of the tube appeared to be 2 crack networks 1/2" and 7/32" long, respectively. These are arbitrarily designated as 1 and 2 in Figure 7-126. The one located 1/4" l

j from the bottom of the tube also appeared to be a doubic crack network (Figure 7-127). ,

7-12 u

l This tube was first cut into pieces A and B, as documented in Figure 7-125, before any axial sectioning was performed. piece A, which 1

contained the defect located 1 5/8" from the top of the tube, was sectioned along the 10' - 190* diameter to bisect the defect. The two j halves were designated as the O' and 180* halves. 1.D. inspection showed l numerous dark spots with a yellowish outline of apparently crystalline i

material and some bright pita in addition to confirming the presence of i

the crack networks described previously. Macro-optical micrographs of the 0.D. and I.D. of piece A after sectioning are presented in Figures 7-128 and 7-129. respectively.

The portion of the crack in the O' half of piece A was pulled open to examine the crack morphology by macro-optical and scanning t

{ electron microscopy. Macro-photographs of the upper and lower fractures i

! (Figures 7-130 and 7-131) show that they are not purely intergranular with ductile failure separating regions of ICA around the entire tube. I The crack documented above shows throughwall ICA, along a circumferential  ;

i length of NO.31". Another region, between areas 7 and 8, shown in the

• SEM fractography of the lower f racture (Figure 7-132), also indicated throughwall ICA. EDS analyses of grain boundary deposits in area 1; j Figure 7-132 indicated sulfur contamination.

The 180' half of piece A was also pulled to expose the crack surfaces for further analysis. Figures 7-133 and 7-134 indicate the j material separation which occurred due to this operation. The crack labeled 2 in Figure 7-126 opened considerably but did not tear into crack

1. Instead, the specimen fractured axially. It is cicar from both macro-optical (Figures 7-134 and 7-135) and SEM studies (Figure 7-136) that this axial fracture was due to ICA which was essentially throughwall for a length of so.4". These figures also provide some indication of the three-dimensional nature of the ICA extending beyond the fracture

] surfaces. Note also (Figure 7-134) that numerous anall I.D. circumferential cracks opened up during pulling. These smaller cracks gave no 0.D.

i' visual indications.

i 7-13

Tube A24-94 (Repair Test)

The 0.D. visual inspection of this tube did not reveal any defects in agreement with the absence of an eddy current indication.

It was sectioned longitudinally along the 90' - 270' diameter to yield the O' and 180* halves, as indicated in Figure 7-137. 1.D. inspection l showed some pitting and regions of discoloration. Both halves were subsequently strained, but the 0* half pulled into 2 pieces along a crack located N3/4" from the bottom before any plastic strain had occurred.

The location of this fracture with respect to the collar is shown in Figure 7-138. This piece was thus divided into 3 sections labeled A, B

& C, respectively (Figure 7-137) so that further evaluation of the fracture faces could be performed. Piece A was "re-strained" to yic1d 10% plastic strain which opened up an I.D. circumferential crack ,

approximately 1/64" long and 1/2" down from the top. Straining the 180' half opened 3 circumferential I.D. cracks between 1/16" and 1/8" long at 2 1/8", 2 7/16" and 2 3/4" from the top of the tube specimen, respectively (Figure 7-139). The longest crack (at 2 1/8") had a corresponding dimple (due to neckdown) on the 0.D. Numerous smaller circumferential cracks were also noted on the 1.D. along the entire length of the strained tube section. Most cracks were associated with regions of discoloration.

Macro-optical micrographs of the fracture surfaces of the crack located 3/4" from the bottom of the tube are presented in Figure 7-140.

The crack appeared to have been I.D. Initiated with throughwall ICA extending over a circumferential distance of 0.15". Figure 7-141 illustrates more clearly that beyond this region of ICA, the fracture mode was ductile. Extensive EDS analyses of grain boundary deposits near the I.D. In areas 4 and 5 are given in Figures 7-142 and 7-143, respectively. Sulfur was present at almost all locations evaluated, with a high Zn concentration at Spot 1, area 5. Na was also detected in area 5 and, in general, the Cr concentrations were high compared to base metal.

7-14

l 1 7.5 Auger and X-Ray Photoelectron Spectroscopy (XPS) Analyses for Sulfur Pickup by New Surfaces of OTSG Tubing l Appendix 9.5 describes in detail the experimental methodology for preparation of ion-implanted sulfur standards, the microanalytical

, procedures for archive tubing as well as the P2D2 C-ring. Following j is a summary.

l 7.5.1 Archive Tubing i,

Archive OTSG tubing samples, which had not been service-exposed j

in the TM1-1 plant, were exposed to a pre-conditioning in loop 3 at elevated temperature in simulated reactor coolant. Auger and XPS studies of these conditioned samples and the standards gave the

following three results.

! 1. The analysis of ion implanted standards showed that Auger electron egectrogeopy can detect quantities of sulfur as low as 3 x 10 g/cm (3pg/ft2) if distributed within the first 10 nm below the surface. If such an amount of sulfur were distributed uniformly through a 100 nm thick region below the j

surf ace, tge total dytectable sulfur content would be j 0.03 ug/cm (30pg/ft ). Amounts lower than that could escape detection.

i

2. The conditioned samples showed significant boron contamin-ation, absent in the standards. The Auger signal for the l

j baron compound (unidentified) consisted of a major peak at 170 eV and a minor peak at 152 eV. The latter may interfere l with the sulfur peak at 148 eV and increase the sulfur levels that can go undetected by a factor of ten or more. No peak overlap occurred in XPS, however, and the XPS detection limit forsulfurwasdeterm{nedtobefivetimesthatofAES,or 0.15 pg/cm (150pg/ft ) within the first 100 nm.

I

3. No sulfur was detected in any of six areas analyzed on conditioned specimens.

Itisgoncludedtgatthosespecimens contained less than 0.15 pg/cm (150pg/ft ) of sulfur within the first 100 nm below the surface and less than 0.015 pg/cm2 r

(15 pa/ft2 ) within the first 10 nm.

i i 7-15 1

7.5.2 C-ring P2D2 The C-ring specimen analyzed was identified as P2D2. It was 4

removed from exposure to primary water during the third cycle. Auger and XPS studies produced the following tesult:

No sulfur was detected at any of the depth icvels analyzed.

l I

Based on the above calibration study with the ion implanted standards, a

the detection limit of elemental sulfur in Inconel Alloy 600 is f 2 0.15 pg/cm in the first 100 nm. It is concluded that the sulfur content of C-ring P2D2 is below that icvel.

7.6 Eddy Current Inspection Results 1

In September,1982, the Field Data Analysis section of

! Westinghouse Nuclear Energy Systems undertook eddy current testing of a number of long term corrosion test tube samples which had been removed from the Three Mile Island (TMI) Unit No. I steam generators.

A baseline multiple frequency eddy current inspection was performed at test frequencies which were specified by GPU-N. A list of tubes which were inspected is contained in Table 7-4. All tubes were eddy current inspected using a dif ferential bobbin probe (diameter 0.052 in.)

j and test frequencies of 45 KHz, 200 KHz, 400 Kilz, and 800 Kitz. All

! signal traces with defect indications can be found in Appendix 9.6.

l The calibration standard consisted of a section of archive j tubing with a 0.052 inch diameter thru-wall drilled hole. The phase angle of the drilled hole was set at 40' for all frequencies. The 400 KHz drilled hole signal is shown in Figure 9-4. A section of OTSG tubing with machined partial ID indications, which was to be used

) for ' repair' tests, was not employed in this phase of the program.

Indications were noted on six tubes during the baseline inspection:

l I

1 f

1 7-16 l

J

_-~- ._ . __ .___ __ . ._

Test Tube Section Indication Run A16-69 (Figure 9- 5) 2"-6 1/2" 95 percent I.D. none A13-63 (Figure 9-6) 20 9/16"-23 9/16" Small dent none A88-7 (Figure 9-7) 2"-9 3/4" 82 percent I.D. 2 A13-63 (Figure 9-16) 11"-18 15/16" <20 percent 0.D. 1 96 percent I.D.

A24-94 (Figure 9-24) 19 5/16"25 7/16" 30 percent 0.D. 1 A16-69 (Figure 9-30) 6 1/2"-12 1/4" 3 l

Additional eod/ current testing was performed upon completion of each cycle of operation of each autoclave loop. A summary of these inspections is also presented in Table 7-4 with further explanation following.

Of all the tubes tested for baseline indications only seven were eventually utilized for the four autoclave test runs (see also Table 6-1); four of them had defects during the baseline inspection, three did not. Test 1 contained tubes A13-63, 11"-18 15/16", and A24-94, 19 5/16"-25 7/16", both with defect indications. Test 2 contained tubes B16-22, 52" to 59", without defect, and A88-7, 2" to 9 3/4", with defect. Test 3 (hydrogen peroxide run) contained only one tube specimen, i.e., A16-69, 6 1/2"-12 1/4", with defect. And finally Test 4 contained tubes A24-94, 36"-42", and B94-27, 4 1/2" to 10 1/2",

both without defect indications. Tube A24-94, piece 6, with a known through wall defect was used in the Leak Rate Experiment. Following is a summary of all inspections for each tube throughout the duration of the experimental runs:

! Test 1:

Tube A13-63, 11"-18 15/16" (Fig. 9-16 to 9-23):

l l This tube showed the same through wall indications throughout l

l all inspections af ter each cycle, HFT through 6.

I Tube A24-94, 19 5/16"-25 7/16" (Fig. 9-24 to 9-31):

l This tubo did not show any change in signal from the baseline inspection, af ter the IIFT and 1st cycles. It had previously shown a 30% 0.D. type indication near the end of the tube; af ter cycle 2 it 7-17 l

t _ _ - - -_

exhibited an additional previously unseen indication. A re-analysis of the eddy current tape recorded during this inspection has shown a number of signals along the length of this tube with an apparent thru-wall indication near the' tube center. It is uncertt.in, from the review of the tape, as to the initiation (0.D. or I.D.) of this indication (Figure 9-27). For the remaining inspections through cycle 6 the indications did not change. Note: This tube had numerous eddy current indications prior to removal from the steam generator.

Test 2:

Tube A88-7, 2"-9 3/4" (Fig. 9-7 to 9-15):

In the baseline inspection this tube had shosn an 82% through wall indication initiating from the I.D. This signal did not change in any of the subsequent inspections af ter the HFT through 6th cycle.

Tube B16-22, 52"-59" (No indication--no tracing)

This tube never showed any eddy current indications from the baseline to the 6th cycle inspection.

Test 3:

Tube A16-69, 6 1/2"-12 1/4" (Fig. 9-32 to 9-38)

In the baseline inspection tube A16-69, 6 1/2" to 12 1/4" -

exhibited an I.D. indication the size of which was difficult to estimate due to a distortion of the signal (Figure 9-32). It is estimated that this indication could be as much as 80 percent through wall.

Subsequent inspections of this tube showed this indication consistently in the range of 60 to 80 percent. This signal never changed throughout all inspections f rom the H 02 2 run through cycle 4.

This was the only tube sample contained in Test 3.

Test 4:

Tube A24-94, 36"-42" (No indication--no tracing), and Tube B94-27,__4 1/2"-10 1/2" (No indication--no tracing): ,

Neither one of these tubes had a baseline eddy current indication. The traces remained essentially unchanged throughout all inspections, HFT through 4th cycle.

7-18

a Leak Rate Test:

1 Tube A24-94, piece 6:

Baseline inspection of tube A24-94, piece 6, was performed on August 2, 1983. It had been supplied for an additional leak rate test which was not in the scope of long-term corrosion tests, and had a known through-wall indication.

7.7 Leak Rate Experiment A detailed description of this experiment can be found in Reference j 4. A section of THI-1 steam generator tubing with a small circum-ferential through-wall crack was supplied by GPU for measurements of leak rates through the damaged area. For the first four runs, leak races varied from near zero (0.027 ml/ min maximum) to about 1.2 ml/ min at 1100 lb. axial load. For Run #5 the maximum load was increased to 1500 lbs. At this load, the leak rate increased to

! 4.73 ml/ min. Subsequent runs resulted in higher leak rates at the lower loads indicating possibly a plastic opening of the defect or flushing of debris during the first 1500 lb application. The average leak rate measurements are tabulated in Table 7-5 and presented in graphical form in Figure 7-144.

Meta 11ographic examination of the crack along with photo-micrographs, SEM and EDS analysis is presented in Figure 7-145 through 7-171. An unabbreviated copy of the Leak Rate Report ( } is included in Vol 2 of this document.

Summarizing, it may be said that the crack was circumferential, fully intergranular and very complex, abo se four timos as long at the I.D. as at the 0.D., and partly three-dimensional. In view of the variable width of the passages, with sone of them being very narrow, possibly producing boundary layer effects, and because of the drastic changes of the flow direction arouad grains, the calculation of an ideal cross section of the crack open to the flow may be a very dif ficult, if not impossible task.

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l 4 i Figure 7-47. Microstructure of Specimen P1Dl, Area B. l f, i 7-66 RH-2882 i

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l i  ! i i i Figure 7-48. Microstructure of Specimen P1D2, Area A.

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 !                                       Figure 7-49.                Microstructure of Specimen PID2, Area B.

i l 7-68 l l RM-2884 l __ _. ___ . _ . _ __ . _ _ _ _

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Tl(y, . sp f.,* 5 - l l j Figure 7-50. Microstructure of Specimen IDS, Area A. il 7-69 RM-2885

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i,,. j Figure 7-51. Microstructure of Specimen IDS, Area B. 7-70 i i RM-2886 l l

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Figure 7-52. Microstructure of Specimen P1A2, Area A. i J

i 7-71 l RH+2H81

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] I'igure 7-53. Microstructure of Specimen P1A2, Area 11. a 7-72 RM-2888 l l

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i i l, Figure 7-54. Microstructure of Specimen PLA3, Area A. I I i i 7-73 4 W 2889

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) Figure 7-55. Microstructure of Specimen PI A3, Area B. I J l

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Figure 7-56. Micrographs of Surface Condition of C-Ring 2154 af ter Exposure ,

)

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m l , i-va.s5i=' A. wx Figure 7-57. Micrographn of Surface Condition of C-Ring P2A4 after Exposure ' I l I 7- 7 f , i RM-6188 1 - - ___ .-_-_- _ =

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I Figure 7-58. Micrographs of Surf ace Conda'an of C-Ring P2D1 af t.cr Exposure 1

!,                                                                                            7-77

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I ) Figure 7-59. Micrographs of Surface Attack at Area A of C-Ring 1B4 after Exposure (100X) I 7-78 l , RM-6390 !

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v f s l Figure 7-60. Micrographs of Surface Attack at Area B of C-Ring IB4 af ter Exposure l 1 i l 7-79 RM-6391

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1 4 ) l 7-114 I RM-3651

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1 Dws. 9366A6) Visually 3 Short Tube A16-69: Examinations Circumferential Crack 1.lke Features

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Figure 7-124. SEM Fractography of Tube A13-63 (Lead Test Specimen) 180* Half, Piece IB, after Breaking Open a Crack 3" from the Top of the Tube. This Piece was not Strained. E a. O v.

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i Figure 7-136. SDI Fractography of Tube A24-94 (Lead Test Secimen) 180* Half, Piece A, after Breaking Open the Crack 1 5/8" from the Top of the Tube. Figure 7-135 j indicates the fracture surface investigated. 7-155 RM-6419

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Figure 7-143. SDf/EDS Analyses of Particulate Material on the Grain Boundaries ) of Area 5 in Figure 7-141. l 7-162 RM-6396

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Figure 7-147. Energy dispersive x-ray spectra (EDS) of the tube OD areas A and B from Figure 7-146. In interpreting these spectra, it should be remembered that the instrument used in this technique is not sensitive to elements with atomic numbers below 11, so that boron, hydrogen and oxygen in the boric acid do not show in the spectra. 7-166 c__.....

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