ML19261B222
| ML19261B222 | |
| Person / Time | |
|---|---|
| Site: | Dresden  |
| Issue date: | 09/30/1978 |
| From: | Webb Patricia Walker GENERAL ELECTRIC CO. |
| To: | |
| Shared Package | |
| ML19261B218 | List: |
| References | |
| NEDC-24143, NUDOCS 7902140255 | |
| Download: ML19261B222 (40) | |
Text
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SEPTEMBER 1978 THIS DOCUMENT CONTAINS POOR QUAUTY PAGES DRESDEN 1 RADIATION LEVEL REDUCTION PROGRAM INTERGRANULAR CORROSION TESTS OF SENSMIZED TYPE-304 STAINLESS STEEL IN DOW NS-1, AND STRESS CORROSION CRACKING TESTS OF TYPE-304 STAINLESS STEEL AND CARBON AND LOW ALLOY STEELS IN DOW COPPER RINSE SOLUTION W. L. WALKER qqo2N GEN ER AL h ELECTRI
NEDC-24143 Class I September 1978 DRF No. 509DEV0021 DRESDEN 1 RADIATION LEVEL REDUCTION PROGRAM INTERGRANULAR CORROSION TESTS OF SENSITIZED TYPE-304 STAINLESS STEEL IN DOW NS-1, AND STRESS CORROSION CRACKING TESTS OF TYPE-304 STAINLESS STEEL AND CARBON AND LOW ALLOY STEELS IN DOW COPPER RINSE SOLUTION W. L. Walker Principal Engineer l$ s' l
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J. C. Danko, Manager Plant Materials and Process Development
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Approved:
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Approved: y
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e G. M. Gordon, Manager
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. Prd ebstle, Manager Plant Materials Engineering Ap lied Metallurgy and Chemistry NUCLE AR ENERGY ENGINEERING DIVISION
- GENERAL E LECTRIC COMPANY SAN JOSE, CALIFORNI A 95125 GENER AL h ELECTRIC
DISCLAIMER OF RESPONSIBILITY This document was prepared by or for the General Electric Company. Norther the General Electnc Company nor any of the contnbutors to this document:
A Makes any warranty or representation. express or Implied, with respect to the accuracy, completanoss. or usefulness of the information containedin this docu-ment. or that the use of any information disclosed in this document may not infringo privately owned ric) hts; or B.
Assumes any responsibility for Isability or damage of any kind which may result from the uso of any Information disclosed in this document.
NEDC-24143 Table of Contents Page ABSTRACT vii 1.
INTRODUCTION 1
2.
SUMMARY
3 3
DETAILED DESCRIPTIONS S
3.1 Test Materials 5
3.2 Test Specimens 5
3.3 Specimen Exposures 7
3.4 Specimen Examinations 8
4.
CONCLUSIONS 10 4.1 General Intergranular Attack 10 4.2 Copper Rinse Solution 10 5.
REFERENCES 29 DISTRIBUTION 31 iii/iv
NEDC-24143 LIST OF ILLUSTRATIONS Figure Title Page 1
Bent Beam Specimen and Stainless Steel Cover Plate Drawing 13 2
Assembled Bent Beam Specimen Pair, with Stainless Steel 14 Cover Plates (scale in photograph is inches) 3 Furnace Sensitized Type-304 Stainless Steel (Heat No. 78500) 15 Bent Beam Specimens (as-polished, 250X) 4 Type-304 Stainless Steel (Heat No. M7616) Welded Pipe 16 Specimens (as-polished, 250X) 5 Type-304 Stainless Steel (Heat No. 2P6396) Welded Pipe 17 Specimens (as-polished, 250X) 6 Type-304 Stainless Steel (Heat No. 2P6426) Welded Pipe 18 Specimens (as-polished, 250X) 7 Furnace-Sensitized Type-304 Stainless Steel (Heat No. 78500) 19 Bent Beam Specimens (oxalic acid etch, 250X) 8 Type-304 Stainless Steel (Heat No, M7616) Welded Pipe 20 Specimens (exalic acid etch, 250X) 9 Type-304 Stainless Steel (Heat No. 2P6396) Welded Pipe 21 Specimens (oxalic acid etch, 250X) 10 Type-304 Stainless Steel (Heat No. 2P6426) Welded Pipe 22 Specimens (oxalic acid etch, 250X) 11 Tensile Surface of Furnace-Sensitized Type-304 Stainless 23 Steel (Heat No. 78500) after Exposure to Dow Copper Rinse 12 Tensile Surface of Furnace-Sensitized Type-304 Stainless 24 Steel (Heat No. 46436) after Exposure to Dow Copper Rinse 13 Tensile Surface of Furnace-Sensitized Type-304 Stainless 25 Steel (Heat No. M3951) after Exposure to Dow Copper Rinse 14 Tensile Surface of Post-Weld Heat-Treated ASTM A336-F1 Low 26 Alloy Steel (Heat No. 43563) after Exposure to Dow Copper Rinse 15 Tensile Surface of Post-Weld Heat Treated ASTM A302-B Low 27 Alloy Steel (Heat No. A5933) after Exposure to Dow Copper Rinse 16 Tensile Surface of Post-Weld Heat-Treated ASTM A106-B Carbon 28 Steel (Heat No. 66549) after Exposure to Dow Copper Rinse v
NEDC-24143 LIST OF TABLES Table Title Page 1
Composition of Type-304 Stainless Steels used in the 11 Investigation of Intergranular Attack by Dow !!S-1 2
Composition of Alloys used in Copper Rinse Investigation 11 vi
N EDC-24143 ABSTRACT Corrosion tests were performed to evaluate the extent of intergranular attack on sensitized Type-304 stainless steel by a proprietary Dow Chemical solvent, NS-1, which is to be used in the chemical cleaning of the Dresden 1 primary system.
In addition, tests were performed to evaluate stress corrosion cracking of sensitized Type-304 stainless steel and post-weld heat-treated ASTM A336-F1, A302-B, and A106-B carbon and low alloy steels in a solution to be used to remove residual metallic copper from the Dresden 1 primary system surfaces following the chemical cleaning.
No evidence of deleterious corrosion was observed in either set of tests.
vil/viii
NEDC-24143 1.
INTRODUCTION A large corrosion test program has been associated with the proposed chemical cleaning of the Dresden 1 nuclear power plant primary system surfaces to reduce the radiation exposure associated with required inspections. The solvent chosen for the cleaning operation was a proprietary compound, NS-1, formulated by the Dow Chemical Company.
A considerable amount of corrosion testing was per-formed by Dow in the process of the development of this solvent (Reference 1).
However, some additional testing was requested by various parties involved in the cleaning program to corroborate the initial findings of Dow, and to evaluate a minor modification of the primary solvent composition for a single special application.
The two primary corrosion concerns associated with NS-1 have been related to general intergranular attack of sensitized Type-304 stainless steel (304 SS) and to stress corrosion cracking er both sensitized 304 SS and plain carbon and low alloy steels. While Dow had evaluated general intergranular attack of sensitized 304 SS in their investigations, it was felt that additional work should be performed using heats of this alloy with known susceptibility to sensitization / stress corrosion cracking, based on tests performed by the General Electric Company's Nuclear Technology Department in other unrelated programs.
An investigation was performed using multiple heats to confirm Dow's observa-tions of lack of evidence of intergranular attack during simulated cleaning cycles in the primary NS-1 solvent, and the results of this investigation are reported in this docament.
The second investigation was prompted by a change in the planned method for control of copper redeposition during the cleaning operation. The initial plan was to remove the copper by an electrolytic process from the circulating solution. However, this proved to involve significant engineering difficulties and a simpler method of removal was developed. By lowering the concentration of the primary solvent, adding hydrogen peroxide (H 0 ),
nd adjusting the 22 pH to a value of approximately 9.5, redeposited copper could be removed quickly at a moderate temperature.
This method was referred to as the " copper rinse."
While no deleterious differences in corrosion of either 304 SS or the plain 1
NEDC-24143 carbon and low alloy steels would have been predicted as a result of these modifications, it was considered prudent to perform confirmatory tests. The results of this investigation are also reported in this document.
2
NEDC-24143 2.
SUMMAP.Y Corrosion investigations were performed to evaluate the general intergranular corrosion behavior of sensitized 304 SS in Dow NS-1, and the stress corrosion cracking behavior of 304 SS and plain carbon and low alloy steels in a proposed copper rinse solution to be used to dissolve any redeposited copper on the Dresden 1 primary system surfaces.
In the general intergranular corrosion investigation, specimens from four different heats of 304 SS were exposed to simulated cleaning cycle conditions and examined for evidencs of intergranular attack. Some specimens were severely sensitized by furnace heat treatment, some were in the as-welded condition, and others were welded and then subjected to a low temperature sensitization heat treatment which produces increased sensitization in the weld heat-affected zone without affecting the adjacent base metal. No indications of preferential intergranular attack were observed, which is consistent with data generated previously by the Dow Chemical Company.
In the copper rinse investigation, stressed creviced bent beam specimens of three different heats of 304 SS and single heats of three plain carbon and low alloy steels were exposed to a simulated rinse solution for four times the anticipated actual cleaning time and examined for evidence of stress cor-rosion cracking. The 304 SS specimens were in the furnace sensitized condition, and the plain carbon and low alloy steels were in the post-weld heat-treated condition. No indications of stress corrosion cracking were observed.
3/4
NEDC-24143 3.
DETAILED DESCRIPTIONS 3.1 TEST MATERIALS 3.1.1 General Intergranular Attack Investigation Test materials for the general intergranular corrosion investigation consisted of four heats of Type-304 SS (M7616, 2P6396, 2P6426, and 78500), with the compo-sitions shown in Table 1.
Three of the heats were in the form of 10-cm (4-in.)
Schedule 80 pipe, and the fourth heat was 15-cm (6-in.) Schedule 80 pipe.
At the time of its selection, heat 78500 was one of the most susceptible heats to intergranular stress corrosion cracking, and was specifically chosen for that reason. However, heat M7616 has also proven to be quite susceptible to intergranular stress corrosion cracking in the as-welded condition 4.n pipe tests. The other two heats were selected because of their ready availability in the as-welded condition at the time of this investigation.
3.1.2 Copper Rinse Investigation Three heats of Type-304 SS and single heats of ASTM A336-F1, A302-B, and A106-B were used in the copper rinse investigation as representative of the principal pressure-containing and structural materials in the Dresden 1 plant. The com-positions of these materials are shown in Table 2.
The 304 SS heats selected were chosen from library materials wh.ch were susceptible to intergranular stress corrosion cracking in the furnace sensitized condition, based on previous testing.
The plain carbon and low alloy steel heats were simply chosen from among those being used in another portion of the Dresden 1 corrosion test program, because there was no prior basis for selection of specific heats.
3.2 TEST SPECIMENS 3.2.1 General Intergranular Attack Investigation Spec' mens used in the general intergranular attack investigation were of two types. The specimens from heat 78500 were rectangular bent beam specimens (Part 1 of Figure 1) which had been subjected to a furnace heat treatment of 50 hours5.787037e-4 days <br />0.0139 hours <br />8.267196e-5 weeks <br />1.9025e-5 months <br /> at 648 C (1200 F) with a furnace cool. These specimens had been 5
NEDC-24143 exposed to a simulated cleaning cycle in "used" NS-1, strained 2% in the outer fibers on constant radius blocks, and then subjected to exposure to simulated BWR service conditions for 11,700 hours0.0081 days <br />0.194 hours <br />0.00116 weeks <br />2.6635e-4 months <br /> at the time of this examination.
A specimen which had seen only demineralized water at the cleaning cycle tempera-ture of 121 C (250 F) and then the BWR exposure was used as a control for this condition.
"Useo" NS-1 consists of the primary solvent with iron and nickel additions in concentrations (1200 ppm and 650 ppm, respectively) anticipated as maximums in the actual cleaning operation.
The specimens from the other three heats were fabricated from as-welded pipe segments, with the inside diameter surfaces grcund after welding. The welding procedure and welding heat input for these specimens was the same as that used in the EPRI pipe tests; 12,200 joules /cm (31,000 joules /in).
Longitudinal segments were cut from each pipe section, with the weld in the approximate center of each segment. One segment from each weld acted as the unexposed control for each heat; one segment was exposed to the NS-1 cleaning cycle in the as-welded condition, and one segment was subjected to a low temperature sensitizing (LTS) heat treatment of 500 C (932 F) for 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> and then exposed to the NS-1 cleaning cycle.
This heat treatment produces severe sensitization in weld heat-affected zones, without sensitizing the adjacent base metal, because of nucleation of carbide precipitates by the welding process. Povich (Reference 2) has demonstrated this in isothermally heat-treated 304 SS, and the same phenomenon has been demonstrated in welded 304 SS by Povich and other General Electric Company investigators in unpublished work.
3.2.2 Copper Rinse Investigation The specimens used in the copper rinse investigation were rectangular cross-section bent beams, with Type-304 SS cover plates to provide a crevice on the tensile surface of the bend, as shown in Figure 1.
Prior to straining on con-stant radius blocks to give approximately 2% strain in the outer fibers, each snecimen was coated with a demineralized water slurry of Fe 0 on the tensile 34 surface to simulate a crud layer. The stainless steel cover plates were installed and the specimens were strained in pairs on stainless steel radius blocks.
An assembled specimen pair is shown in Fi ure 2.
6 6
NEDC-24143 Quadruplicate specimens from each heat of material were tested. The stainless steel specimens were sensitized by heat treating for 40 hours4.62963e-4 days <br />0.0111 hours <br />6.613757e-5 weeks <br />1.522e-5 months <br /> at 620 C (1150 F) in an air atmosphere, followed by air cooling.
The low alloy and carbon steels were given a simulated p u t-weld heat treatment of 3 hours3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> at 620 C in air, followed by an air cool.
33 SPECIMEN EXPOSURES 3.3.1 General Intergranular Attack Investigation The solution to which all specimens were exposed consisted of Dow NS-1 with iron and nickel additions to simulate the levels anticipated during the actual cleaning cycle at the Dresden 1 plant. The work performed previously by Dow indicates that iron additions increase the corrosivity of the NS-1 solvent, so the tests represent a conservative position.
Exposure times for all tests were approximately 100 hours0.00116 days <br />0.0278 hours <br />1.653439e-4 weeks <br />3.805e-5 months <br /> at a temperature of 121 C (250 F) in a static TFE fluorocarbon-lined autoclave, with a solution volume-to-surface ratio of approximately 4 ml/cm (1 gal /ft ).
As stated previously, the specimens from heat 78500 had accumulated a total of 11,700 hours0.0081 days <br />0.194 hours <br />0.00116 weeks <br />2.6635e-4 months <br /> subsequent simulated BWR exposure at the time of their examination for purposes of this investigation. Specimens from the other three heats were examined following only the NS-1 exposure. The specimens from heat 78500 were exposed in a special run during 1976 as part of the initial investigation into the effects of NS-1 on the subsequent service behavior of Type-304 stainless steel. The specimens from the other three heats were exposed during the last mixed alloy run in the fracture mechanics test program on carbon and low alloy steel-clad cracks.
332 Copper Rinse Investigation The teat solution consisted of a 5% solution of Dow NS-1, without the inhibitor, adjusted to a pH of 9 5 with ammonium hydroxide (NH 0H) and with hydrogen peroxide 4
(H 0 ) added af ter the pH adjustment to give a concentration of 0.25 wt%.
All 22 exposures were performed in plastic beakers in a constant temperature bath at a temperature of 43 C 1 5 C (110 F 2 10 F), with a single pair of specimens 7
NEDC-24143 in each beaker. The specimens were submerged completely in 750 ml of solution in the beaker, givint a solution volume-to-surface area ratio of approximately 3 ml/cm2 (0.7 gal /ft ),
2 The testing was performed in two runs with half of the specimens from each heat tested in each run. While the proposed rinsing time for the copper removal step in the Dresden 1 cleaning operation is approximately 6 hours6.944444e-5 days <br />0.00167 hours <br />9.920635e-6 weeks <br />2.283e-6 months <br />, the stress corrosion. cracking tests were conducted over periods of 24 and 23 hours2.662037e-4 days <br />0.00639 hours <br />3.80291e-5 weeks <br />8.7515e-6 months <br />, respec-tively, in order to maximize the probability of the occurrence of stress corrosion cracking. Temperature variations were less than + 2 C (5 F) in both runs, and fresh test solution was prepared for each run.
3.4 SPECIMEN EXAMINATIONS 3.4.1 General Intergranular Attack Investigation All specimens were mounted and polished for metallographic examination. On heat 78500 the surface examined was the tensile surface of the specimens, while the inside diameter surfaces in the weld heat-affected zones were examined on the welded specimens from the other three heats. Photomicrographs from each specimen in the as-polished condition are shown in Figures 3 through 6.
No indications of intergranular attack were observed on any specimen exposed to NS-1.
The specimens were then given a light electrolytic oxalic etch to delineate sensitized grain boundaries, and the results are shown in Figures 7 through 10.
All specimens gave indications of significantly sensitized microstructures.
3.4.2 Copper Rinse Investigation Following the test exposure, the specimens were removed from the radius blocks and cleaned ultras- -ically in alcohol. The tensile surface of each specimen was examined througn a binocular macroscope at a magnification of 30X. No indications of stress 2orrosion cracking were observed on any of the specimens, although most specimens exhibited rupture of the heat-treat oxide film from plastic straining during the loading operation.
8
NEDC-24143 All specimens were then subjected to destructive metallographic examination.
A 2.5-cm (1-in.) section was cut from the center of each specimen, mounted and polished, and examined for indications of stress corrosion cracking at magnifications up to 200X. No indications of stress corrosion cracking were observed, ar.d there was no evidence of localized intergranular attack on the stainless steel specimens. Photomicrographs from typical specimens are shown in Figures 11 through 16.
9/10
NEDC-24143 4.
CONCLUSIONS 4.1 GENERAL INTERGRANULAR ATTACK The results of this investigation confirm the work previously performed by Dow Chenica2 :ompany, and indicate that exposure to Dow NS-1 cleaning solvent does not cause intergranular attack of sensitized Type-304 stainless steel under the conditions established for the cleaning operation.
4.2 COPPER RINSE SOLUTION The data generated in this investigation do not indicate that the proposed copper rinse step represents a significant risk from the standpoint of stress corrosion cracking of severely sensitized Type-304 stainless steel or post-weld heat-treated low alloy and plain carbon steels.
11
NEDC-24143 Table 1 COMPOSITION OF TYPE-304 STAINLESS STEELS USED IN THE INVESTIGATION OF INTERGRANULAR ATTACK BY DOW NS-1 Heat No.
C Mn P
S Si Ni Cr M7616 0.063 1.71 0.024 0.012 0.54 10.4 18.8 2P6396 0.057 1.69 0.028 0.023 0.59 10.3 10.7 2P6424 0.074 1.63 0.024 0.013 0.46 9.7 18.5 78500 0.045 1.63 0.019 0.013 0.53 9.0 19.1 Table 2 COMPOSITION OF ALLOYS USED IN COPPER RINSE INVESTIGATION Alloy Heat No.
C Mn P
S Si Mo Cr Ni 304 78S00 0.045 1.63 0.019 0.013 0.53 19.05 9.00 304 46436 0.07 0.86 0.022 0.013 0.64 0.40 18.65 8.27 304 M3951 0.057 1.66 0.023 0.014 0.44 18.83 10.42 A336-F1 43563 0.24 0.76 0.018 0.031 0.24 0.48 0.12 0.16 A302-B A5933 0.23 1.37 0.005 0.012 0.23 0.60 A106-B 66549 0.26 0.81 0.012 0.028 0.19 Notes:
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Bent Beam Specimen and Stainless Steel Cozer Plate Drawing 13
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Bent Beam Specimens. (As-polished,250X) 15
NEDC-24143 AS WE LD ED
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Type 3&S Stainless Steel (Heat No. M7616) Welded Pipe Specimens. (As-polished,2 SOX) 16
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NEDC-24143 AS POLISHED 250X
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NEDC-24143 5.
REFERENCES 1.
Technical Study for the Chemical Cleaning of Dresden 1, Dow Chemical Company, DNS-D1-016, June 15, 1977.
2.
Povich, M.
J., Low Temperature Sensitization of Type-304 Stainless Steel, Corrosion, Vol. 34(2), February, 1978.
29/30
NEDC-24143 DISTRIBUTION Name M/C L. D. Anstine V04 R. L. Cowan 138 J. C. Danko 407 W. R. Dehollander 110 J. S. Gay 888 B. M. Gordon 138 G. M. Gordon 138 R. B. Hamilton 853 J. H. Holloway 585 R. A. Proebstle 146 W. H. Reas V04 C. P. Ruiz V04 W. L. Walker 407 D. E. Wax V17 NED Library (5) 328 VNC Library V01 EXTERNAL DISTRIBUTION T. D. Boyce (DNS)
C. F. Cheng (ANL)
D. E. Harmer (DNS)
W. I. Kiedaisch (CECO)
T. Y. Moon (DNS)
G. L. Redman (CECO)
R. W. Staehle (0.S.U.)
G. P. Wagner (CECO)
J. L. White (CECO) - 15 31/32
GEN ER AL h ELECTRIC