ML20149F993
| ML20149F993 | |
| Person / Time | |
|---|---|
| Site: | Perry  |
| Issue date: | 01/29/1988 |
| From: | CLEVELAND ELECTRIC ILLUMINATING CO. |
| To: | |
| Shared Package | |
| ML20149F991 | List: |
| References | |
| NUDOCS 8802180054 | |
| Download: ML20149F993 (200) | |
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{{#Wiki_filter:n FINAL Rt. PORT 4 MAIN STEAM ISOLATION VALVE SOLENOID VALVE FAILURE ANALYTICAL CHEMISTRY RESULTS January 29, 1988 8802100054 880212 gDR ADOCK 050 g 0 File No. 8702342M Notebook Ref.: 20294, p. 106
TABLE OF CONTENTS Section Page I. Executive Summary 3 Introduction 3 Analysis Plan 3 ! Obser va tions 4 Conclusions 4 II. Root Cause Hypotheses 5 Statement of Hypotheses 5 Sequence of Analysis 5 Analytical Methodology 6 Analysis Results 7 Evaluation of Results 8 III. Summar y 12 ; Table I 13 I Diagram I 15 Diagram II 16 APPENDIXIS 1 i , Appendix At Gas Chromatographic Analysis of Instrument Air Samples [ for Fesidual Hydrocar bons Appendix B: Analytical Repor t - Instrument Air f Appendix C: Hardness of 0-rings Appendix D: Hardness of Valve Seats Appendix Et Compr ession Set of 0-r inge Appendix F: Main Steam Isolation Valves - Nondestructive Evaluation by Optical Microscopy Appendix G: Main Steam Isolation valves ring Destructive ! Evaluation by Scanning Electron Microscopy l Appendix H: Main Steam Isolation Valves - Energized Elastomer Seats '
- Destructive Evaluation by Scanning Electron Microscopy Appendix I Infrared Examinations of 0-rings from MSIV Units Appendix J: Thermal Examinations of 0-r ings from Control MSIV Units
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SECTION I Executive Summary Introduction This repor t summarizes the analytical investigar'on of the Main steam Isolation valve (MSIV) Pilot Solenoid f ailure, w.rtch caused the MSIV's to fail a fast closur e test on November 3,1987. The pur pose of the investigation was to determine the reason the EPDM exhaust por t seats did not release from the exhaust por t when the pilot solenoids wer e de-energized. Elastomer par ts from failed, nonf ailed, and "never used" pilot solenoid valves were examined. Two components, o-r ings and elastomer exhaust por t seats, from each of the solenoid valves were examined. The instrument air supply to the containment building, to the solenoid and to the two inch actuator line were analyzed for the pr esence of hydrocar bons. The o-rings and the exhaust por t seats are composed of EPDM rubber , and wer e both in contact with br ass valve components. They were t exposed to the same instrument air and at the same temperatur e. The investigation focused on the o-r ings (vs. the elastomer seats) because of their accessibility and advanced degr ee of degr adation. Changes occurring at the o-r ing ar e consider ed compar able to changes ' occurring to the elastomer seats. Two hypotheses were proposed as causes for the MSIV f ailur e. The fir st hypothesis proposed that a hydrocar bon contaminant in the instr umen t air supply af fected the o-r ings and seats. The second hypothesis proposed that excessive heat caused degradation of the EPDM rubber which changed its proper ties and caused the f ailur e of the valve. Analysis Plan The approach to determining the cause of the failure included both nondestr uctive and destructive tests. All nondestructive tests were per formed fir st to minimize loss of limited sample. These tests included:
- 1) Optical Microscopy to record the appearance of the components,
- 2) Gas Chromatography analysis of the air supply,
- 3) Hardness and Compr es sion Set of the o-r ings and/or seats * .
record physical changes in the samples. Page 3 of 16
Once these results were reviewed, the de s tr uc tive tests wer e per for med. These included:
- 1) Inf r ar ed Spec tr oscopy of the o-rings to identify chemical changes,
- 2) Scanning Electron Microscopy and Energy Disper sive X-ray microanalysis to record physical and elemental differences between the o-rings and seats, and
- 3) Thermal analysis of a control o-ring to determine the effects
>f temper atur e.
Differences between the failed, nonfailed and "never used" valve components wer e compar ed. Observations Physical Changes The compr ession set and har dnes s of the o-r ing s and seats pr ogr essively incr ea sed from con tr ol to nonfailed to failed valve components. This indicated that the EPDM componen ts became less elastic. The indentations in the energized elastomer seats wer e deeper in the failed MSIV valves than in the nonfalled valves. The outside (100-150 micr ome ter s) layer of the failed o-ring had changed and appeared mor e porous than the outside layer of either the nonf ailed or control o-r ing. Chemical Changes Sever al (3) failed o-rings showed evidence of a stear ate mater ial on their sur f ace . Copper and oxygen wer e pr e sen t on the sur f ace and 100-150 micc ome ter s into the interior of the f ailed o-r ings. Copper was also pr esent on the sur f ace of the failed seats. Conclusions Ins tr ument air analysis for hydr ocar bon s indicated only tr ace levels, far below concen tr a tions considered to be harmful to EPDM material. Fur ther , analysis of the EPDM materials from the pilot solenoids pr ovided no indication that high levels of hydrocar bons wer e pr esent to attack the o-rings and elastomer seats. Both the chemical and physical changes which did occur to the o-r ings and seats could be explained by the pr esence of excessive heat (Hypo thesis 2) . At higher temper a tur es , the EPDM material will sof ten which would allow a deeper indentation to occur in the seats. Higher temper a tur es would also encour age chemical interactions between the EPDM and the br a ss valve body . The temper a tur e and the pr obable presence of a stear a te compound on the valve seats could result in some bonding which would retard the operation of the valves. Page 4 of 16
i l l 1 1 Root Cause Hypotheses
SECTION II Root Cause Hypotheses Statement of Hypotheses Hypothesis 1 The fir s t hypothesis states that a contaminant in the ins tr umen t air could have affected the EPDM o-r ings and elastomer seats within the f ailed valves. If hydrocar bons wer e pr esent, they would absor b into the EPDM, making it spongy. If the ins tr ument air contained significant quantities of hydrocarbons, all of the MSI pilot solenoids j would have been exposed. The hydr ocar bons would not induce migr ation 1 of copper or oxygen into the EPDM ma ter ial . If a solid material contaminated the ins tr umen t air, an accumulation of these par ticles , would be expected on the o-r ings and at the elastomer seats. Hypothesis 2, The second hypothesis states that elevated temperatures af fected the EPDM mater ial of the o-rings and elastomer seats in the f ailed valves. The elevated temper a tur es changed the EPDM material, causing the j elastomer seats to stick to the br as s valve body. Physical and chemical changes would have occur r ed at both the o-ring and the I elastomer seats. Interactions between the br ass and the rubber would ' be possible if temper a tur es wer e high enough to cause the components i in the EPDM formulation to migrate. l l Sequence of Analyses l The study was organized into two basic types of analyses: nondes tr uc tive and des tr uc tive . The nondes tr uctive tests wer e per formed fir st, to minimize the loss of limited sample. Once these r esults wer e reviewed by CEI per sonnel, decisions wer e made on how to proceed. The destructive tests wer e fir st per formed on the o-r ings, and then on the seats. Three types of samples were compared: components from a f ailed valve, a nonfailed valve, and a "never used" control, the investigation focused on the o-rings (vs. the elastomer seats) because of their accessibility, lar ger sample size and advanced degree of degradation. Changes occur r ing at the o-rings wer e believed to be correlate to changes occurring at the elastomer seats. A few tests were also performed on the solenoid valve bodies. The in s tr umen t air was sampled at the following locations: the air supply to the containment building, the air supply to the solenoid, and the air supply to the two-inch actuator line. Table I lists the samples, identifications, descriptions and the applied analysis methods. Samples MSIV24, 27, and 28 wer e identified by CEI as components removed fr om "failed" pilot solenoid valves. Sample MSIV26 was identified as components from a pilot solenoid which was in ser vice, but did not fail. Page 5 of 16
Within the main steam isolation valve pilot solenoids, two component types wer e examined. The fir st was the o-rings. The o-ring was determined to be EPDM, which was compr essed between two components of the brass pilot solenoid valve body (see Diage ams I & II). The second compoment was an clastomer seat, which provided the sealing sur f ace at the exhaust por t when the pilot solenoid is energized. The seats were also composed of EPDM, and wer e in constant contact with the br ass cone-shaped exhaust por t , within the same pilot solenoid body as the o-r ings (Diagrams I & II). The o-rings and seats, having endured the same physical service conditions within the same valve bodies, were consider ed to be of equal value for evidence of' failur e mechanisms. The o-r ing s have mor e sur f ace ar ea in contact with the br ass valve body. They are also compr essed between two metal sur f aces to form a seal. Therefore, they wer e considered to be advanced cases of elastomer degradation providing dir ec t evidence to root cause. The o-r ing s , however, are a passive component of the pilot solenoid, and their degr aded condition did not contr ibute to the f ailur e of the seat to release from the exhaust por t or ifice when the solenoid was de-ener g ized. Analytical Methodoloay Gas chromatography was used to evaluate the quality of the instrument compr essed air system. Samples of compr e ssed air from the Plant system wer e collected and submitted for analysis to de ter mine if hydr ocar bons wer e pr e sen t , which could have caused elastomer degr adation, leading to sluggish valve per formance. Durometer hardness tests wer e conducted. The elastomer hardness is an impor tan t proper ty in valve applications. The elastomer must be sof t enough to conform and ther eby seal pneumatic por ts. The hardness test measures the resistance to indentation which is dependent on elastomer modulus and viscoelasticity. Compr e s sion set was evaluated. The compr ession set test is intended to me asur e the ability of an elastomer to retcin elastic pr oper ties after pr olonged compr ession. Elastomer s in valve applications must be resilient enough to "take up the slack" due to thermal expansion / contr action of valve components and provide an ef fective seal. Optical and scanning electron microscopy were used to examine physical (mor pholog ical) changes which occur r ed to the o-rings and seats. Ener gy disper sive x-r ay microanalysis spectroscopy (EDS ) was used to examine chemical changes which occur r ed at specific locations in the sample. The exter ior sur f aces of the seats and o-r ings wer e examined using the above mentioned technique s . In order to examine in ter ior changes, cross-sections of the samples were also prepared and the same techniques wer e applied. Inf r ar ed spec tr oscopy (IR) was used to examine var ious EPDM o-rings from var ious MSIV pilot solenoids. The pur pose of the examinations was to detect possible chemical changes which might be related to the f ailur e of elastomer seats to release from exhaust por ts of pilot solenoids when de-energized. Page 6 of 16
Dif fer ential scanning calor ime tr y (DSC) and thermal gr avimetr ic analyses (TGA) wer e conducted. The thermal characteristics of virgin (con tr ol) o-r ings wer e investigated by these techniques. The pur pose of the investigations was to determine the ther mal stability of the 0-rings and the ef fect of copper on this stability. Analysis Results Gas Chromatography No significant quantities of condensable hydr ocar bons wer e found within the instrument air (Appendixes A & B). Durometer Hardness Tests 0-rings and valve seats from oper ational MSIV26 were slightly harder than unused rings and seats. However , o-r ing s and valve seats fr om failed MSIV24, 27, and 28 wer e significantly har der than unused coun ter par ts (Appendixes C & D). Compression Set 0-r ings from oper ational MSIV26 displayed very little compr ession set. However , o-r ings fr om failed MSIV24, 27, and 28 had significant compression set (Appendix E). Optical Microscopy The o-rings fr om the failed pilot solenoid valves (MSIV24, 27, 28) have flattened and ar e mor e br ittle than the nonfailed (MSIV 2 6 ) or control o-r ings (Appendix F, Figur es 9, 10 & 12). Within the f ailed valves, the rubber o-r ings have adher ed to the br ass of the valve body itself (Appendix F, Figure 13) . The exhaust por t seats fr om the failed pilot solenoids have an indentation which is deeper than the nonfailed seat (Appendix H, Figur e 8) . Scanning Electron Microscopy / Energy Disper sive X-r ay Microanalysis A significant quantity of copper can be found on the failed o-ring sur f ace , as well as pene tr a ting 100-150 micr ometer s into the failed o-r ing s (Appendix G, Tables I & II). A secondary layer has formed on the outside of the failed o-rings. This layer, in addition to containing copper, is mor e por ous and contains oxygen (Appendix G, Figur es 13, 17, 19). The amount of calcium is significantly less in the failed and nonfailed o-rings (MSIV24, 26, 27, & 28) than in the control (Appendix G, Tables I & II). Page 7 of 16
More copper is present at the sur f ace of the indentation of the failed seats than in the nonfailed and con tr ol seats (Appendix H, Table I, Figur e 6) . No mor phological changes have occur r ed to the rubber beneath the indented areas of the seats (Appendix H, Figures 10 & 14). ) Infr ar ed Spectroscopy Several of the o-r ings have stearate based organic acid calts such as calcium stear ate on their sur f aces. Excessive levels of an or ganic - acid salt at the sur f ace of the o-r ing is believed to be the result of heat on the EPDM (Appendix I, Page 2). , Stearate salts at temper a tur e s above 250 F would liquefy and when , cooled, could act as a glue between the EPDM and the br ass valve body (Appendix I, Page 3). Thermal Analysis The EPDM thermal analysis results show that a weight loss degr adation begins near 300 C (572 F). No significant change in this degr adation temper a tur e was obser ved when the o-r ing s wer e allowed to be in contget with copper metal. Additional exper imen ts (DSC) to 200 C (392 F) showed no evidence for a catalytic effect of copper on th'. oxidation of the o-rings. In the abgence of copper , the o-rings sbo< evidence of oxidation near 270 oC (518 F) (Appendix J, Page 2) . The above exper iments wer e dynamic in that a temper a tur e incr ease of either 10 or 20 / minute was used. As a result, the above tests ar e very acceler ated and pr ovid e little information as to the long- ter m stability of the o-r ings. Evaluation of Results There are two possible explanations for the failure of the solenoids to pr ovide sufficient air flow to the MSIV s to allow adequate rapid closur e times. The two hypotheses, stated br iefly, ar e Hyp tnesis It Contaminants f r om the air system wer e absor bed by the EPDM, which caused a significant change in its elastomeric proper ties. Or, contaminants from the air system deposited in the valve which caused physical jamming. Hypothesis II: The solenoids wer e exposed to some sor t of a transient elevated temper atur e, which resulted in elastomer degr adation. Ricerca per formed physical and chemical tests on the failed, nonfailed and "never used" o-r ings and elastomer seats. We drew conclusions as to the cause of failure based on observations fr om bo th EPDM o-r ings and EPDM valve seats. Failur e of the valve was caused exclusively by degradation of the seat. However, as stated ear lier , valuable and pa-allel information can be dr awn from the obser vations of changes to the o-rings, since the o-r ings wer e subjected to the same environment as the seat. Page 8 of 16
*%s All the ovidence generated suppor ts the second hypothesis for tailur e.
Namely, excessive heat cauced a degr adation of the EPDM components in the failed valves. No evidence was observed which would suppor t the contaminated air hypothesis (Hypo the sis 1). The results and their implications are discussed in the next two sections. Instrument Air Contamination (Hypothesis M Ther e was some question regarding possible contaminants in the ins tr ument air and their contr ibution to the f ailur e of the ela s tomer s . No par ticulates wer e found on the o-r ings or seats which could cause a physical jamming of the valve mechanisms. This ef fectively eliminates airborne par ticulates as a cause. The extensive elemental analyses which wer e per for med on the EPDM ma ter ials involved did not disclose any elements associated with the introduction of hydr ocar bons . If hydr ocar bon contaminants wer e present, a "leaching pr oce s s" would occur by absorbing and desorbing cycles. Mater ial muld then be expected to migr a te from the EPDM rubbers. This leaching process could cause the EPDMs to har den. The spectral results show no evidence for unexpected hydrocar bons on any pieces removed from service. silicon lubr icants wer e pr esent. But, no foreign hydr ocar bons wer e pr e sen t on elastomer sur f aces or on r esidual EPDM material scr eped from the valve bodies. In GC analyses per formed on ins tr umen t air, hydr ocar bon levels wer e very low. Hydr ocar bons wuld be suspected of causing oil components within the EPDM to migr ate but not neces sar ily induce migration of a mater ial such as the calcium stearate. Hydrocar bone # ail to explain either the observations abou t copper or oxygen, or why the most extensive degradation occur r ed in por tions of the par ts physically in contact with the valve body. In fact, mor e sever e degr adation was obser ved in those areas most pr o tec ted fr om hydr ocar bons in the air. This is exactly the opposite from what we would expect if contamination of the plant air wer e the sour ce of the f ailur e. In short, no analytical results or service circumstances suppor t EPDM failur e as a result of hydrocar bon attack. Elastomer Degr adation Due To Elevated Temper ature (Hypothesis M While no analytical results suppor t the attack of elastomer material by hydr ocar bon contaminants, all obser va tion s suppor t f ailur e as a result of heat degradation. Evidence suppor ts this f ailur e mode in the form of embr i t tlemen t , cr ack ing , and physical adher ence of the elastomer par ts to the metal valve bo d y . This evidence is corroborated by the severe physical and morphological changes observed in elastomere from the failed pilot solenoids. Both phys cal and i chemical evidence also suppor ts copper catalysis as a contr ibutor to elastomer degr adation. Page 9 of 16
Evidence from Valve Seats The EPDM valve seats actually provide the sealing sur face in the valve body. Valves failed because the seats adhered to the valve body and prevented air flow. We observed all of the. same degr adation characteristics in the valve 3 seats that we saw in the o-rings. Likewise, we found a buildup of copper in the por tion of the valve seat which was in direct contact with the sealing area. The elastomer seats fr om the thr ee failed solenoids exhibited an incr ease in dur ome ter hardness. Based on actual plant per for mance , this incr ea se in the hardness of seats corr elates ' to, a loss of solenoid per for mance . As observed in the o-rings, the same type of calcium depletion from the in ter ior of the seats and resultant buildup of s tear ate on the sur f aces was discovered. The last major obser va tion is that the indentation in the valve seats is in direct cor r elation with the per formance of that valve seat. The gr ea ter the indentation (usually called compr e ssion se t) the poorer the per for mance of the solenoid valve. However, the seats fr om a given valve wer e not degraded as badly as tne cor r esponding o-r ings. If heat alone was responsible for degradation, seats and o-rings should be -degr aded equally. This difference in degradation suppor ts copper catalyzed oxidation as an impor tant effect that occur s after temper a tur e excur sions. The difference in degradation is a result of the ratio between the area of elastomer in contact with the br ass valve body to to tal elastomer in a par t. The o-rings had a large por tion of its sur f ace in contact with the br a s s , while the seats did not. This allows a higher por tion of the o-r ing elastomer to undergo degradative oxidation reactions. Ef fects Expec'ted from Elastomer Oxidation When ' oxidation occur s in an elcstomer ma ter ial, bonds ar e br oken and bonds ar e reformed. When a mechanical for ce is applied to an elas tomer ma ter ial, the rubber part can be de for nied . Normally when the mechanical force is released, the par t r e tur ns to its original s h a ps'. But, if the elastomer is locked in a deformed state when oxid69on occur s, the par t may be permanently deformed. 5^fter chemical degradation, adhesion can develop between an elastomer and a solid pressed againte it. All solids have roughness. The valve bodies in this case show machining mar ks so there is cer tainly some roughness associated with the metal. The longer an elastomer is pressed against the metal, the more probable it is that some adhesion will occur . This is par ticular ly tr ue if either oxidation reactions are occur r ing or if for mula tion ingr edien ts ar e migr a ting to the sur f ace of the elastomer . m Page 11 of 16 l
l Evidence from 0-r ings The o-rings removed from failed valve bodies showed significant morphological (cr acking , as well as adhesion to the valve body), chemicaA and physical changes. The chemical changes included l migration of copper into the fir s t 100-150 micr ome ter s wher e the 1 o-r ings contacted the valve body. In this layer, there was a buildup of oxygen which is chemically attached to the elastomer. Depletion of calcium level from within the body of the o-r ing was obser ved. The j sur face of the o-ring shows the pr esence of stear ate salt. Stearates ar e common components of EPDM r ubber s. The only sour ce of copper was from the br ass valve body itself. Metallic copper is not pr one to , migration through ela s tomer s . It must have been removed chemically i from the valve body as a salt and then diffused through the rubber. 1 The buildup of stear ate salts on the sur f ace of the rubber and the loss of calcium from within tne rubber, can be explained by calcium stearate diffusing to the sur f ace of the o-r ing. Af ter tr ace amounts of etching of the br as s body occur r ed , copper stearates could form which wer e fr ee to back diffuse into the rubber. The rate of this phenomenon would be str ongly governed by temper a tur e . At higher temper a tur es , faster diffusion takes place, the more likely the etching of the br as s , and subsequent back migration of the copper stear ates will occur . Physical testing of the o-rings has shown that their measur ed dur ome ter hardness incr eased as a function of degradation. That is, the wor se the physical appearance of an o-ring and the poorer the per formance of the valve in service, the higher the durometer hardness measur ed. This physical result fits with the observations above. One of the po s sible functions of calcium stearate in an elastomer formulation is to provide internal lubr ication or to mildly soften the mater ial. If a substantial por tion of the stear ate has migrated to the sur f ace , the par t would be expected to harden. The pr esence of oxygen in the sur f ace of the failed o-r ings would be consistent with a hardening of this sur f ace. Oxidation of elastomer s makes them harder and mor e br ittle. Brown et.al. investigating the Brunswick shut down have concluded that some EPDM for mula tion s undergo rapid exothermic reactions in the pr esence of oxygen and copper. Copper is a well-kno wn catalyst for organic reactions and it fr equen tly has been used to catalyze oxidation types of reactions. He did find a higher level of copper in the failed samples ver sus the nonfailed samples. Higher levels of copper existed in the most degraded areas of failed o-r ings , specifically the sur f ace 100 micr ometer s. The excess copper in these severely degraded elastomer regions correlates well with observed oxygen content in these same ar eas . Ther efor e , it is reasonable to conclude from all of the evidence that copper was involved in a catalytic oxidation process. Page 10 of 16
V e
.O Summary I,
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SECTION III Summar y We believe that f ailur e resulted from the following sequence of events: a) The valves which failed experienced an excur sion above their rated use temper a tur e . Without this excur sion, the ensuing events would either not have occurred or would have taken much longer to occur . b) S tear ate salts, most pr obably the calcium salt, migrated to the sur f ace of the elastomer much more rapidly than normal due to the high temper atur e. c) Copper salts der ived from ver y minor attack on the valve body diffused back in to the elastomer. The salt was most pr oba bly copper stearate. d) Oxygen from the air in the valve diffused through the elastomer and caused oxidation reactions of the elastomer. These oxidation r eactions wer e most probably catalyzed by copper . e) As a result of the oxidation reactions, the elastomer lost its "rubber-like" pr oper ties. This could have caused it to stick to the valve seat. f) When solenoid pr es sur e was removed fr om the seat, it failed to draw back from the valve body and allow adequate air flow to actuate down str eam equipment. I l Page 12 of 16 L-
TABLE I Sample Date/ Time Descr iption Analysis MSIV10 11/7/87:0730 PS 2-F 5 56: Ins tr . GC Air at containment Pene tr ation (ou t side) , 10 min. blow down, 15 min. purge of sampler MSIV11 11/7/87:0745 PS2-F556: In s tr . GC Air at containment P ene tr a tion (outside) 10 min. blow down, 15 min,. purge of sampler MSIV20 11/16/87:1600 B 21-F0 28 D: Solenoid IR, OM valve body MSIV21 11/16/87:1600 B 21-F022 A: Solenoid IR, OM valve body (test solenoid) MSIV22 11/16/87:1600 B 21-F 028 A: 0-r ing , CS, H, IR, elastomer seat & OM MSIV24 11/16/87:1600 B21-F0 28B: 0-r ing , CS, H , OM, elastomer seat SEM/EDX,
& IR MSIV25 11/16/87:1600 B 21-F0 22C: 0-r ing , CS, H, OM, elastomer seat & IR MSIV26 11/16/87:1600 B21-F0 28 C: 0-r ing , CS, H , OM, elastomer seat SEM/EDX,
& IR MSIV27 11/16/87:1600 B-21-F02 2D: 0-r ing , CS, H , OM, elastomer seat SEM/EDX,
& IR l
MSIV28 11/16/87:1600 B-21-F02 8 D: 0-r ing , CS, H, OM, elastomer seat SEM/EDX,
& IR MSIV Control ---
Never Used CS, H , OM, 0-r ing, elastomer SEM/EDX, seat IR, & T , MSIV33 11/30/87:2200 B 21-F0 22B: I ns tr . GC l Air grab sample l from 2" supply l l Page 13 of 16 L
TABLE I (co n t ' d) Sample Date/ Time Descr iption Analysis
- MSIV34 11/30/87:2215 B 21-F0 22B: I n s tr . GC Air grab sample
- from solenoid supply line
*The abreviations used to identify the analysis were as follows:
GC - Gas Chromatography; CS - Compr ession Set; H - Hardness; OM - Optical Microscopy; IR - Infrared Spectroscopy; T - Thermal Analysis; SEM - Scanning Electron Microscopy; EDX - Energy Disper sive X-r ay Analysis t l l l l l Page 14 of 16 i
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IO.~ Oi . APPENDIX A Gas Chromatographic Analysis of Instrument Air Samples for Residual Hydrocar bons
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l-t TO: J.J. Grimm - CEI FROM: G. E. Walls DATE: November 13, 1987
SUBJECT:
GAS CHROMATOGRAPHIC ANALYSIS OF INSTRUMENT AIR SAMPLES FOR RESIDUAL HYDROCARBONS OVERVIEW The quality of the Perry Nuclear Power Plant in s tr umen t compressed air system is maintained in accordance with a number of technical specifications. One specification states that the air system shall not contain hydr ocar bons in excess of 1 ppm, quantified as methane. Dur ing a recent NRC inspection at the Plant, one or more air-actuated valves failed to operate pr oper ly. T wo samples of compr essed air fr om the Plant system wer e collected and submitted for analysis to determine if hydr ocar bons wer e pr esent. RESULTS Noncondensable Hydrocar bons Sample Time Area e
.pom MSIV-10 1.54 min. 148,714 10.4 Condensable Hydrocar bons 12.91 min. 10,226 0.7 MSIV-ll Noncondensable Hydrocar bons 1.54 min. 123,689 8.7 2.58 min. 2,250 0.2 Condensable Hydrocar bons 12.92 min. 5,756 0.4 7528 Auburn Rcod a Box 1000. Po;nesvitle. Ohio 44077 216/357-3303
Page 2 ~~' J.J. Grimm {UCS; u November 13, 1987 o CONCLUSIONS The results repor ted for condensable hydr ocar bons are based on the chromatographic peak at 12.9 minutes exclusively. The fact that this peak occur s in the standard and blank, as well as in the samples, suggests the possibility of a chr oma togr aphic anomaly rather than the pr e sence of a hydr ocar bon . For this reason, the r epor ted values of 0.7 ppm and 0.4 ppm for condensable hydr ocar bons in samples MS IV-10 and MSIV-ll, respectively, should be considered maximums rather than absolutes. It is my judgment that the in str umen t air samples submitted are, in fact, "clean" with respect to your specification. PREPARATION AND ANALYSIS A gas chr oma togr aphic system was assembled consisting of the following: GC: Varian 3760-5407 Detector: Flame ionization Injector: Heated, flash vaporizing Column: 18' x 3/16" OD stainless steel packed with SP-2100, 20% , on Chr omosor b P, AW, DMCS tr ea ted , 60-80 mesh. Data System: Var ian DS-654 Gas chromatogr aphic operating conditions wer e as follows: Injector Temp: 250 C Detector Temp: 30g C Column Temp: 50 C at injegtion, hold 2 min g at 50 C, progr am 10 pgr min, to 200 C, hold 3 min. at 200 C Carrier Gas: Heljgm at 40 mL per min. FID Electrometer: 10 amps per mv Injection: 2.5 mL gas Preparation of Calibration Standard Master Standard: Methane in Nitrogen, 1.000% (vol.) Scott Specialty Gases Troy, Michigan 48083
h Pace 3 J."J. Grimm " ' ' '". ' " *
' '(
November 13, 1987
- . A 250 ' mL gas sample tube was purged with dry, hydrocar bon fr ee nitr ogen for 10 minutes. Using a gas tight syr inge , 2.5 mL of master standard were injected into the ' gas sample tube.
Concentration: 1% x 2.5 mL 250 mL = 0.01%
= 100 ppm A second 250 mL gas sample tube was pur ged with dr y, hydrocar bon free nitrogen for 10 minutes. Using a gas tight syringe, 2.5 mL-of the 100 ppm standar d wer e injected into the gas sample tube.
Concen tr a tion: 100 ppm x 2.5 mL 250 mL = 1.0 ppm A third 250 mL gas sample tube was purged with dry, hydr ocar bon free ni tr ogen for 10 minutes. This sample represented a blank for instr ument calibr ation. Calibration 2.5 mL 1.0 ppm methane standard analyzed using conditions above. Result: Chromatogr aphic peak at 1.55 min. Peak ar ea 28,832 2.5 mL blank nitrogen standard analyzed using conditions above. Result: Chromatographic peak at 1.51 min. Peak area 14,609 Calibr ation Factor (CF) = 1 ppm (28,832-14,609)
-5
= 7.03 Sample Analysis Peaks Detected Time Ar ea FBIV-10 1.54 min. 148,714 12.91 min. 10,226 158,940 CF x 158,940 = 11.2 ppm, v/v, total hydrocar bons i
Page 4 J . J . Gr imm November 13, 1987 bbCOICd ! " Peaks Detected Time Area MSIV-ll 1.54 min. 123,689 2.58 2,250 12.92 5,756 131,695 CF x 131,695 = 9.3 ppm, v/v, total hydrocar bons Peaks Detected Time Ar ea Lab Air Lab-48 Ricerca HQ l.54 116,747 12.89 11,295 128,042 CF x 128,042 = 9.0 ppm, v/v A ttachmen ts: 1) Chromatogram of calibration standard
- 2) Chromatogr am of nitrogen blank
- 3) Chromatogr am of sample MSIV-10, Atten: 16
- 4) Chromatogr am of sample MSIV-10, Atten: 128
- 5) Chromatogr am of sample MSIV-ll, Atten: 16
- 6) Chromatogr am of sample MSIV-ll, Atten: 64
- 7) Chromatogr am of labor ator y air r
b q u< gens F ,b rf.- <.f nL Greg'ory E. Walls jsb Atts, i File No.: 8702037G Notebook Ref. : 20342-41/56-58 Reviewed By: . l1JCL
/ U ,
s' ri
CHART SPEED 1.I CM/MfN # TTMCNAMT h ATTEN: 16 ZERO: .5% 1 MIN / TICK PACC I
~
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- 12. sos W! As,e
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13.7ee M
Ll3$RLMULQYlg LCIVET:lB7L4MA#9 CHANNEL: 1A-1 T8TLE: HC ZN PERRY PLANT COMP A8R 13:27 7 NOV 07 SAMPLE: 1 PPM CH4 METH00: HYDROC-3 CALCULAT2CN: A% - ANALYS - OP PEAK PEAK RESULT TIME TIME AREA SE? .W1/2 NO NAME AREA % (MIN) 0FFSET COUNTS CODE (SEC) 1 METHANE 57.9002 1.550 0.000 28832 88 8.00 2 36.5150 12.909 18163 BB ? 18.75 3 5.5848 13.700 2781 BB 11.00 > TOTALS: 100.0000 49795 DETECTED PKS: 3 REJECTED PKS: 0 DIVISOR: 1.00000 AMT STD: 1.00000 MULTIPLIER: 1.00000 NOISE: 12.6 0FFSET: 1960 NOTES: COL: 18' X 3/15' 00 SS, 20% SP-2100 HELIUM CARRIER GAS AT 40 ML PER MIN INJECTOR TEMP 250' i DETECTOR TEMP 300* ELECTROMETER 10-12 AMPS PER MV. COLUMN TEMPS 50', HOLO 2 MIN, 10' PER MIN TO 200'
** G C SYSTEM 3750-5407 *+
CHART-SPEED 1of CM/M8N 8 TTNCNAAEAJ7" h ATTEN:- 18 ZERO: 5% I MIN / TICK f/70s /
}
METHANE 1.513 v EL s . s [- , l1 i I 12.see wt.as.e m enemme s
~ +
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- _ 18.FT4 t 3
ma'4me 1 ]
, - ~ , . . . . . . . - - - - . . _ - . - _- . , . , . - _ , - . _ _ . , , _ , , , . , , - - - . -- , . - . . . -, - , - - , , - , ~ - , - - - - -
;y CHANNEL: 1A - I T8TLE: HC IN PERRY PLANT COMP A8R 13:59 7 NOV 87 l SAM?LE: HOUSE N2'BLX METHOD: HVOROC-3 CALCULATf0N: A2 - ANALYS - OP l
PEAK PEAK RESULT TIME TIME AREA SEP W1/2 l NO NAME AREA % (MIN) 0FFSET COUNTS CODE (SEC) . 1 METHANE 59.5742 1.513 -0.037 14609 BB 7.06 l 2 41.4258 12.908 10332 BB 7 20.19 TOTALS: 100.0000 -0.037 24941 DETECTED PKS: 3 REJECTED PKS: 1 DIVISOR: 1.00000 AMT STO: 1.00000 MULTIPLIER: 1.00000 NOISE: 12.5 0FFSET: 1940 NOTES: COL: 18' X 3/16' 00 SS, 20: SP-2100 HELIUM CARRIER GAS AT 40 ML PER MIN INJECTOR TEMP 250' DETECTOR TEMP 300' ELECTROMETER 10-12 AMPS PER MV, COLUMN TEMP: 50', HOLO 2 MIN, 10' PER MIN TO 200'
- 6 C SYSTEM 3760-5407 *+
firrMCHMLAST $
' CHART SPEED 1.1 CM/ MIN F564 /
ATTEN: 16 ZERO: 5% 1 MIN / TICK
~
l I METHAHE. g, egg W.e.e
~
1 l 22.9e9 W1.as.e
-19.016 ut.12.s -
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CHANNEL: 1A - 1 T8TLE: HC ZN PEREV PLANT CCMPR. A8R 14:31 7 NOV 87 SAMPLE 3 M S I U - 10 METHOD: HVOROC-3 CALCULAT20N: A% - ANALYS - 0F PEAK PEAK RESULT TIME TIME AREA SEP U1/2 NO NAME AREA % (MIN) 0FFSET COUNTS C00E (SEO) 1 METHANE 38.7865 1.538 -0.002 148174 EB 6.55 2 2.6759 12.909 10225 BB 7 22.50 3 58.5346 19.015 223605 BB 7111.00 TOTALS: 100.0000 -0.002 382005 DETECTED PKS: 3 REJECTED PKS: 0 DIVISOR: 1.00000 AMT STO: 1.00000 MULTIPLIER: 1.00000 NOISE: 5.7 0FFSET: 2007 NOTES: COL: 18' X 3/16' 00 SS, 20: SP-2100 HELIUM CARRIER GAS AT 40 ML PER MIN INJECTOR 250", DETECTOR 200" FID ELECTROMETER 10-12 AMPS PER MV. COL TEMP: 50", HOLD 2 MIN, PROG 10' PER MIN TO 200' *
** G C SYSTEM 3760-5407 **
POST RUN: SAVE FILE: RAW HYOPC3017
s M Y TMCHNED 7* & CHART. SPEED ~ l.1 CM/ MIN- Pf/6E / ATTEN: 128 ZERO:- 5:: 1 MIN / TICK
._7 Y
METHAHE .530 wins,e l 1 x f f 12.ses , WI.as.e -
- 19.eks wt. e -
i TT*.12 uH f
--,,--m- , - -, , . . , , , - . , . ----. , , ,_.--_.,_-,n-_.. ... , - -,. , , , - - , _ . - - - - - - . - . , - . . , , ,,-.e, --..,n, -,,
eeseswtrarvsasu- mwu r CHANNEL: lA - 1 TITLE: HC IN PERRY PLANT COMPR. AIR 14:31 7 NOV 97 SAMPLE: M S I V - 10 METHOD: HYOROC-3 CALCULATION: A% - ANALYS - OP PEAK PEAK RESULT TIME TIME AREA SEP Ul/2 NO NAME AREA % (MIN) 0FFSET COUNTS CODE (SEC) 1 METHANE 39.5970 1.538 -0.002 148174 BB 6.55 2 2.7327 12.909 10226 BB ? 22.50 3 57.6703 19.016 215005 BB 7111.C0 TOTALS: 100.0000 -0.002 374205 I U Y3TED PMS: 3 REJECTED PKS: 0 OIVISOR: 1.00000 AMT STD: 1.00000 MULTIPLIER: 1.00000 l NOISE: 5.7 0FFSET: 2007 NOTES: COL: 18' X 3/16' OD SS, 20% SP-2100 HELIUM CARRIER GAS AT 40 ML PER MIN INJECTOR 250', DETECTOR 300* . FID ELECTROMETER 10-12 AMPS PER MV. COL TEMP: 50", HOLD 2 MIN, PROG 10' PER MIN TO 200" +
++ 6 C SYSTEM 3750-5407 ++
MTYncHurAJ7 @ CHART SPEED .1.1 CM/MfN EDE/ ATTEN: 16 ZERO: 5% 1 MIN / TICK
~
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l'
~
1 i METHANE __ 1.542 Est.8
~
2.579 1 l
~
t f 12.925 1 .l 1 i
- 23. $1 24.95.
W! 16.8 - t t
CHANNEL: 1A-I TITLE: HC IN PERRY PLANT CCMPR. A8R. 15:02 7 NOV B7 SAMPLE: M S I U - 11 METHOD: HYOROC-3 CALCULAT8CN A3 - ANALVS - CP PEAK FEAK RE5 ULT TIME TIME AREA SE? W1/2 NO NAME AREA 7. (MIN) CFFSET COUNTS C00E (SEC) 1 METHANE 29.5798 1.542 0.002 123589 ES 6.53 2 0.5381 2.579 2250 E9 7 8.44 3 1.3755 12.925 5755 BV 7 15.55 4 63.7159 18.883 266430 VV 7 16.63 5 4.7896 18.952 20028 V8 7 TOTALS: 100.0000 0.002 418153 DETECTED PKS: 5 REJECTED PKS: 0 OIVISOR: 1.00000 AMT STO: 1.00000 MULTIPLIER: 1.00000 NOISE: 4.6 0FFSET: 2011 NOTES: COL: IS' X 3/'B' 00 SS, 20% SP-2100 HELIUM CARRIER 6AS AT 40 ML PER MIN INJECTOR 250', DETECTOR 300' FID ELECTROMETER 10-12 AMPS PER MV. COL TEMP: 50', HOLO 2 MIN, PROG 10' PER MIN TO 200* *
** G C SYSTEM 3750-5407 **
POST RUN: SAVE FILE: RAW HYGFC30lG l l I
M TTncNAAEA)W h _ CHART ~ SPEED 1.1 CM/ MIN PNGC /
-ATTEN: 64 ZERO. 5% 1 MIN / TICK METHANE 1.542 HT;e.e - f
~
2.579 32.925 I j' , 1 4 3 I i
- ,13.083 y 10.f:2 -
W1i36.0
RECALCULATE ON F8LE: HVDPC3015
' CHANNEL: lA - 1 T8TLE: HC 8N PERRV PLANT COMPR. AfR 15:02 7 WCV 97 SAMPLE: M S I V'- 11 METHOD: HYDROC-3 CALCULATION: A% - ANALYS - CP FEAK PEAK RESULT TIME TIME AREA SEP U1/2 NO NAME AREA 7. (MIN) 0FFSET COUNTS COCE (SEC) 1 METHANE 29.5799 1.542 0.002 123689 BB 6.63 2 0.5381 2.579 2250 BB 7 8.44 3 1.3765 12.925 5755 BV 7 16.56 4 63.7159 18.883 266430 VV 7 16.63 5 4.7896 18.952 20028 VB ?
TOTALS: 100.0000 0.002 418153 DETECTED PKS: 5 REJECTED PXS: 0 DIVISOR: 1.00000 AMT STD 1.00000 MULTIPLIER: 1.00000 NOISE: 4.6 0FFSET: 20I1 NOTES: COL: IS' X 3/16' OD SS, 20% SP-2100 HELIUM CARRIER GAS AT 40 ML PER MIN INJECTOR 250', DETECTCR 300* FIO ELECTROMETER lt 12 AMPS PER MV. COL TEMP: 50', HCLD 2 MIN, PROG 10" PER MIN TO 200* *
*+ 6 C SYSTEM 3760-5407 ++
.s
MTTMcHMCA.W $ CHART SPEED 1.1 CM/M2N Pnot /
.ATTEN: 16 ZERO: 5% ! MIfi/ TICK 1
METHANE 1.544 Ea8.0
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SAMPLE: LAB AIR METHOD: HYOROC-3 CALCULAT80N: A8 - ANALYS - OP
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PEAX PEAK RESULT T!ME TIME AREA SEP ul/2 NO- NAME AREA: (MIN) 0FFSET COUNTS CODE (SEC) 1 METHANE 91.1767 1.544 0.004 115T47 EE 6.S3 2 8.8213 12.891 11295 BB ? 17.94 TOTALS: 100.0000 0.004 128042 DETECTED PXS: 2 REJECTED PKS: 0 DIVISOR: 1.00000 AMT STO: 1.00000 MULTIPLIER: , 1.00000 NOISE: 4.6 0FFSET: 1985 NOTES: COL: 18' X 3/16' 00 SS, 20% SP-2100 HELIUM CARRIER 6AS AT 40 ML PER MIN INJECTOR 250', DETECTOR 300* FID ELECTROMETER 10-12 AMPS PER MV. COL TEMP: 50', HOLO 2 MIN, PROG 10' PER MIN TO 200* *
** 6 C SYSTEM 3760-5407 ++
POST RUN: SAVE FILE: RAW HYOPC2019
!DMICit i i
APPENDIX B Analytical Repor t - Instrument Air
F f TO: '^ J . J . Gr imm - CEI FROM - - G. E. Walls i DATE: '?t December 4, 1987
SUBJECT:
ANALYTICAL REPORT - INSTRUMENT AIR 7 INTRODUCTIdN A recent malfunction of one air -oper a ted solenoid valve again raised ' suspicions of hydr ocar bon contamination in the Plant ins tr umeh t air system. Two air samples, collected by you, wer e analyzed by gas-chromatography to determine if hydrocar bons wer e present. Samples MSIV-33 11/30/87 2200 Ricerca Number B 21: F0 2 2B , Instrument Air 20342-042-10 at 2" Supply Line (Gr ab Sample) MSIV-34 11/30/87 2215 Instrument Air at Solenoid Supply '
., 20342-042-20 r>ine: B21: f 02 2B (Grab Sample) s
- .N RESULTS '
~
Nonc6ndensable Hydrocar bons Sample Time- ' Area Epm 20342-042-10 1.38 min. 177,682 11.6 Condensable Hydrocar bons 7.89 min. 9,037 0.6 Noncondensable Hydrocar bons 20342-042-20 1.39 min. 156,885 9.5 1.78 min. 11,778 0.7 Condensable Hydrocar bons 7.89 min. 16,227 1.0
-t-e 7528 Auburn Road . Box 1000. Poinesde. Ohc 4.1077 216/357-3300 a
J.J. Grimm D ccmbcr 4, 1987 CONCLUSIONS Ricerca.hh The results r epor ted for condensable hydr ocar bons ar e based on the chromatographic peak at 7.89 minutes exclusively. The fact that this peak occur s in the standard and blank, as well as in j the samples, suggests the possibility of a chr oma togr aphic ! anomaly rather than the pr e sence of a hydr ocar bon . For this reason, the r epor ted values of 0.6 ppm and 1.0 ppm for . condensable hydr ocar bons in samples 20342-042-10 and 1 20342-042-20, respectively, should be consider ed maximums r ather than absolutes. It is my judgment that the ins tr umen t air samples submitted ar e , in fact, "clean" with respect to your specification. PREPARATION AND ANALYSIS A gas chr omatogr aphic system was assembled consisting of the following: GC: Var ian 3760-5407 Detector: Flame ionization Injector: Heated, flash vaporizing Column 18' x 3/16" OD stainless steel packed with SP-2100, 20% , on Chr omosor b P , AW, DMCS tr eated, 60-80 mesh Data System: Var ian DS-654 Gas chromatogr aphic operating conditions were as follows: Injector Temp.: 250 C Detector Temp.: 300gC Column Temp.: 100 C at injgetion, hold 2 mig, at 100 C, program 10 pgr min. to 230 C, hold 3 min. at 230 C Carr ier Gas Helgm at 45 mL per min. m FID Electrometer: 10~ amps per mv Injection: 2.5 mL gas Preparation of Calibration Standard i Master Standard: Methane in Nitrogen,1.000% (vol . ) i Scott Specialty Gases l , Troy, Michigan 48083 l ) A 250 mL gas sample tube was purged with dr y, hydr ocar bon fr ee I nitrogen for 10 minutes. Using a gas tight syr inge , 2. 5 mL o f master standated were injected into the gas sample tube. Concen tr a tion: 1% x 2.5 mL 250 mL = 0.01%
= 100 ppm
Pcgo 3 J . J . Gr imm December 4, 1987 _ _ , PJcercat inc. A second 250 mL gas sample tube was purged with dry, hydrocarbon free nitrogen for 10 minutes. Using a gas tight syr inge , 2.5 mL
- of the 100 ppm standard were injected into the gas sample tube.
Concen tr ation: 100 ppm x 2.5 mL 250 mL = 1.0 ppm A thir d 250 mL gas sample tube was pur ged with dr y, hydr ocar bon free nitr ogen for 10 minutes. This sample represented the blank for instr ument calibr ation. ATTACHMENTS
- 1. Chromatogram of calibration standard
- 2. Chromatogram of nitrogen blank
- 3. Chromatogram of sample 20342-042-10
- 4. Chromatogram of sample 20342-042-20 During our telephone ' conver sation of Dec. 3, 1987, you expr essed an in ter es t in the chr oma togr aphic peak a retention time 7.9 minutes. Please let me know if you would like us to attempt to identify it by GC-MS.
/ ey t.
Grego y E. Walls jsb Atts. File No.: 8702173G Notebook Ref.: 20342-42 Reviewed By:'fx A! "/Z IM M l')
~;;< -.
D rTMCNMCAJV~~7/ PMGC / W 2. CHAP.T SPEE0 9.9 CM/ MIN ATTEN 16 ZERO: 5% 1 MIN / TICK
~
1 ese METHANE g .),372 W!st.9 - j l
- I k
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- 1s: 3f3 l v
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RECALCULATE ON FILC: TOTAL-HC010' I#d CHANNEL: IA-1 T!TLE: HC IN PERRY PLNT 8NST A8R 9:15 3 CEC 67 SAMPLE: 1.0 PPM STD METHOD: TOTAL-HC CALCULATION: A% - ANALYS - CP PEAK PEAK RESULT TIME TIME AREA SEP W1/2 NO NAME AREA % (MIN) 0FFSET COUNTS CODE (SEC) 1 1.78 1.068 3767 BV 6.81 2 1.28 1.212 2706 VV 7 5.56 3 METHANE 18.95 1.372 -0.048 40177 V8 7.06 4 4.18 7.883 8856 88 19.31 5 3.52 14.411 7459 BV 4.88 6 4.08 14.512 8653 VV 7 2.94 7 4.34 14.612 9195 VV 7 2.94 8 4.54 14.712 9620 VV 7 3.00 9 4.62 14.910 9796 VV 7 3.00 10 4.63 14.911 9822 VV 7 3.00 11 4.65 15.011 9954 VV 7 5.69 12 4.66 15.110 9873 VV 7 5.63 13 4.68 15.211 9924 VV 7 5.81 14 4.67 15.310 9911 VV 7 6.00 15 4.77 15.411 10124 VV 7 6.06 16 4.79 15.510 10149 VV 7 6.00 17 4.71 15.610 9981 VV 7 6.00 18 4.51 15.709 9560 VV 7 6.39 19 4.19 15.809 8889 VV ? 6.13 20 3.97 15.910 8418 VV 7 6.19 21 2.51 16.006 5313 VB 7 6.38 TOTALS: 100.00 -0.04S 212047 CETECTED PKS: 21 REJECTED FKS: 0 DIVISOR: 1.00000 AMT STO: 1.00000 MULTIPLIER: 1.00000 NOISE: 13.7 CFFSET: 2743 NOTES: COL: 18' X 3/15' OD SS, 20% SP-2100 HELIUM CARRIER 6AS AT 45 ML PER MIN INJECTOR TEMP 250* i DETECTOR TEMP 300^ ELECTROMETER 10-12 AMPS PER MV./ 2.5 ML INJECTIONS COLUMN TEMP: 100', HOLD 2 MIN, 10* PER MIN TO 230"
** G C SYSTEM 3760-5407 **
M 2% e PMC / O f C. CHART SPEED 0.9 CM/ MIN ATTEN: 16 ZERO: 5% i MIN / TICK 1 es, wl.a.e - 3,3g3 F 1
- l
( 7.ssA WI.16.0 9 A A. Ate gggggfCL)f
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RECALCULATE ON FILE: TOTAL-HC011 086E S ## O-- CHANNEL: 1A-1 T8TLE: HC 8N PERRV PLNT 8NST A8R 9: 49 3 OEC 67 SAMPLE: NIT. BLANK METHOD: TOTAL-HC CALCULATION: A% - ANALYS - CP PEAK PEAK RESULT TIME TIME AREA SEP W./2 NO NAME AREA % (MIN) 0FFSET COUNTS CODE (SEC) I 1.73 1.059 3559 BV 6.88 2 1.49 1.213 3064 VV ? 7.56 3 3 METHANE 11.99 1.361 -0.059 24739 VB 5.69 4 4.17 7.694 0605 BB 16.19 5 3.94 14.508 8132 VV ? 6.25 6 2.95 14.609 6075 VV ? 4.63 7 5.94 14.709 12257 VV 7 4.69 8 4.87 14.807 19048 VV ? 6.69 9 4.98 14.907 10273 VV 7 6.94 10 5.12 15.007 10559 VV 7 6.94 11 5.17 15.107 10667 VV 7 7.13 12 5.22 15.207 10775 VV 7 7.19 13 5.32 15.307 10955 VV 7 7.19 14 5.36 15.407 11059 VV ? 7.19 15 5.36 15.507 11050 VV 7 7.19 16 5.20 15.605 10730 VV 7 7.44 17 4.89 15.705 10091 VV 7 7.30 18 4.53 15.805 5334 VV 7 7.38 19 4.20 15.906 6673 VV ? 7.44 20 2.40 16.002 4960 VB ? 7.44 21 5.16 22.932 10553 69 ? 55.00 TOTALS: 100.00 -0.059 206267 DETECTED PKS: 22 REJECTED PKS: 1 DIVISCR 1.00000 AMT STO: 1.00000 MULTIPLIER: 1.00000 NOISE: 13.7 0FFSET: 2404 NOTES: COL: 18' X 3/16' 00 SS, 20% SP-2100 HELIUM CARRIER SAS AT 45 ML PER MIN INJECTOR TEMP 250' i DETECTOR TEMP 300* ELECTROMETER 10-12 AMPS PER MV./ 2.5 ML INJECTIONS COLUMN TEMP: 100', HOLO 2 MIN, 10' PER MIN TO 230'
** G C SYSTEM 3760-5407 ++
R rTt1 CHM CN Y 3 Pn&& I of .2 CHART SPEED 0.9 CM/ MIN ATTEN: 16 ZERO: E% 1 MIN / TICK ,
~ s METHAHE 2.380 1
)
l 2 7.886 W1 8.0 F,26.0 26.332 18.243 _ _g
- 23 444 W!i32.0
~
i: RECALCULATE ON F8LE: TOTAL-HC012 8/TCEEE $1 (7/P d2. CHANNEL: 1A-1 T8TLE: HC 8N PERRY PLNT INST A8R 10:20 3 DEC 67 SAMPLE: 20342-042-10 METHOD: TOTAL-HC CALCULATION: A% - ANALYS - CP PEAK PEAK RESULT TIME TIME AREA SEP W1/2 NO NAME AREA % (MIN) 0FFSET COUNTS CODE (SEC) 1 METHANE 72.99 1.380 -0.040 177602 BB 5.88 2 3.71 7.886 9037 BB ? 14.06 3 3 13.14 15.628 31992 BB 7128.00 4 1.52 16.332 3696 BB ? 23.69 5 0.57 18.143 1638 BB 6.56 6 7.96 23.444 19383 BB ? 59.13 TOTALS: 100.00 -0.040 243428 DETECTED PKS: 6 REJECTED PKS: 0 DIVISOR: 1.00000 AMT STO: 1.00000 MULTIPLIER: 1.00000 NOISE: 13.7 0FFSET: 2177 NOTES: COL: 18' X 3/16" 00 SS, 20% SP-2100 HELIUM CARRIER 6AS AT 45 ML PER MIN INJECTOR TEMP 250' : DETECTOR TEMP 300* ELECTROMETER 10-12 AMPS PER MV./ 2.5 ML INJECTIONS COLUMN TEMP: 100', HOLD 2 MIN, 10' PER MIN TO 230'
** G C SYSTEM 3760-5407 **
M77McNMLINr h/ ^ PfrG E / cf G. CHART SPEED 0.9 CM/ MIN ATTEN'2 16 ZER0t. 5% 1 MIN / TICK wtis.o METHANE 3.396 _ _ a.7s3 wi.2... P l 4 k
- 7.893 L
e f pqAtoA.qq LCU8 j
~~'
/AJd I* i
._7_ s.e92
[ T.T. 3 2 . 0 22.967 ] wt 64.eet1iOH 4
RECALCULATE ON F8LE: TOTAL-HC013 8/RIdI' 52 dh# d2- ' CHANNEL: 1A-1 T2TLE: HC 2N PERRY PLNT INST A2R 10:53 3 DEC 67 SAMPLE: 20342-042-20 METHOD: TOTAL-HC CALCULATION: A% - ANALYS - OP PEAK PEAK RESVLT TIME TIME AREA SEP W1/2 NO NAME AREA % (MIN) 0FFSET COUNTS CODE (SEC) 1 METHANE 19.34 1.386 -0.034 156885 8V 5.69 2 1.45 1.783 11778 V8 7 11.63 3 2.00 7.893 16227 88 15.75 4 0.76 14.408 6202 8V 7 31.00 5 1.47 14.510 11954 VV ? 4.88 6 1.62 14.611 13179 VV 7 5.94 7 2.18 14.711 17706 VV ? 6.19 8 1.88 14.806 15218 VV ? 7.44 9 1.91 14.907 15504 VV 7 7.50 10 1.94 15.007 15700 VV 7 7.50 11 1.96 15.106 15884 VV ? 7.75 12 1.98 15.205 16035 VV ? 7.75 13 2.01 15.308 16345 VV ? 7.08 14 2.00 15.405 16214 VV ? 7.75 15 1.97 15.505 15995 VV ? 7.75 16 1.91 15.606 15515 VV ? 8.06 17 1.82 15.704 14797 VV ? 8.00 18 1.73 15.804 14036 VV 7 8.06 19 1.67 15.906 13525 VV ? 8.05 20 1.34 16.002 10876 VV 7 7.75 21 2.26 16.091 18300 V8 7 22 44.79 22.907 363406 GB 7:30.44 TOTALS: 100.00 -0.034 811285 DETECTED PKS: 22 REJECTED PKS: 0 DIVISOR: 1.00000 AMT STO: 1.00000 MULTIPLIER: 1.00000 NOISE: 13.7 0FFSET: 2295 NOTES: COL: 18' X 3/16' OD SS. 20% SP-2100 HELIUM CARRIER GAS AT 45 ML PER NIN INJECTOR TEMP 250' : DETECTOR TEMP 300' ELECTROMETER 10-12 AMPS PER MV./ 2.5 ML INJECTIONS COLUMN TEMP 100'. HOLO 2 MIN, 10' PER MIN TO 230'
++ G C SYSTEM 3760-5407
Ricerca I. ... APPENDIX C Hardness of 0-rings l l l l
l i TO: J . J . Gr imm - CEI l FROM: G. G. Sweetapple DATE: December 14, 1987
SUBJECT:
HARDNESS OF 0-RINGS Twelve used . o-r ings and four unused o-r ing s wer e analyzed for S hor e A hardness using the Shore Micro 0-ring Hardness Tester , Model 714M. The calibr ation of the microtester was verified with seven ASTM D2240 standards. Samples wer e mounted n in a 0.07 inch o-ring fixtur e, conditioned and tested at 22 + 0.5 C. Both sides of the used o-r ing s were measur ed due to visual differences obser ved . Four readings of each o-r ing side wer e made; the mean value and standard deviation are summar ized below. - Shore A O-r ing B Hardness (Mean) (SD) Unused #1 77.5, 78.0* 0.5, 0.7*
#2 77.5, 77.8* 1.1, 0.4*
#3 78.5, 79.0* 0.9, 0.7*
#4 78.2, 78.5* 0.4, 0.5*
MSIV 22 #1 Side A 96.0 0.7 Side B 87.2 1.9 MSIV 22 #2 Side A 94.0 0.7 Side B 88.8 0.8 MSIV 24 #1 Side A 88.8 1.3 Side B 89.0 1.6 MSIV 24 #2 Side A 89.8 0.8 Side B 92.2 1.3 MSIV 25 41 Side A 80.8 0.4 ; Side B 82.2 1.1 i MSIV 25 #2 Side A 83.2 0.8 Side B 81.0 0.7
- Retested on 12-14-87 Initial Test 12-6-87 ,
t i i , l I f 7528 Auburn Rood . Boa 1000 Po nesWe ONo 4077 i 216/357-3300 !
Page 2 IbC ei U- - J. J. Grimm December 14, 1987 O-r ing ID Hardness (Mean) _(SD) MSIV 26 il Side A 81.2 0.8 Side B 82.8 0.8 MSIV 26 42 Side A 80.8 1.1 Side B 81.0 1.6 MSIV 27 il Side A 84.8 0.8 Side B 94.0 2.3 MSIV 28 42 Side A 95.5 1.6 Side B 91.0 1.6 NOTE: MSIV 27 42 and MSIV 28 41 were not tested. One inch o-r ings from stock #1465253. %;A E k,' ., Gar y G. Sweetapple jsb File No.: 8702145 Notebook Ref.: 12907-71 Reviewed By: W. R. Bramstedt R. L. Cryberg
$5$k1% %
QJ Fr [l' d4' ' r
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[YCQi'Ci, ' APPENDIX D Hardness of Valve Seats
h 6 TO: J. J. Grimm - CEI FROM: G. G. Sweetapple DATE: December 14, 1987
SUBJECT:
HARDNESS OF VALVE SEATS Seven used valve seats and four unused valve seats (f r om '
$1465253) wer e analyzed for Shore A hardness with the - shore mict odur ome ter . Calibtation was verified with seven ASTM D-2240 stagdards. The samples wer e conditioned and tested at 22 +
0.5 C. Used valve seats were analyzed on the "active" sur f ace 7 car e f ully avoiding ar eas of compr e s sion set as sho wn in figur e . below. Four measurements of dif ferent spots were made on each ! seat; the mean hardness and standard deviation are summar ized below. ! v v i I t Seat ID Shore A Hardness (mean) (SD) Unused il 83.5, 83.0* 0.5, 0.7*
#2 83.8, 83.2* 0.8, 0.8* '
#3 84.0 0.7 .
64 83.8 0.8 MSIV 22 85.2 0.4 " MSIV 24 85.5 1.'l MSIV 25 84.5 1.1 . MSIV 26 83.8 0.8 MSIV 27 85.5 0.9 MSIV 28 85.5 1.1 ,
- Retested 12-14-87 !
Initial Test 12-6-87 l 1-
%% i Gar y' G. S wee pple (UMe [ [ g, Reviewed By: W. R. Bramstedt R. L.fyberj f Notebook Ref.: 12907-72 752s Avoun. noco . Bon 1000. Po nessefomo 44377 2te/357 3330 File No.: 8702197 i
-- - . - - -. .e , - - - ,
i [O C C ; s ,' l l 1 APPENDIX E Compression Set of 0-rings I
4 TO: J . J . Gr imm - CEI FROM: G. G. S weetapple DATE: November 24, 1987 S UBJECT: COMPRESSION SET OF 0-RINGS Four teen used- o-rings wer e measur ed for existing compr ession set per ASTM D-395. Six unused o-rings wer e measured to calculate. the original thickness. Four measurements were made on each o-r ing and aver aged. Compr ession set was then calculated using the formula: C 3= [( to- t i) + to ) x 100% C is compression set as a percent of original thickness tb is the average original thickness ti is the average final thickness i Sample Compr ession Set, % MSIV 22 61 17.3
#2 15.8 MSIV 24 #1 21.9
#2 16.2 MSIV 25 #1 12.2
#2 11.1 MSIV 26 41 9.5 62 9.4 MSIV 27 f1 16.5
#2 17.2 FSIV 28 #1 23.4
#2 14.1 If you have any questions about this wr k, please call me at 357-3256.
6$hyk Gary G. Sweetapple jsb Reviewed By: O b b' Notebook Ref.: 12907-68 7528 Auburn Rood
- Bom iCOO . Po nehire. ONo 44077 File No.: 8702125 216/357 3300
} Ct i APPENDIX F Main Steam Isolation Valves - Nondestructive Evaluation by Optical Microscopy
6 TO: FROM: J. J . Gr imm - CEI K. A. Kr u tyholowa DATE: December 1, 1987
SUBJECT:
MAIN STEAM ISOLATION VALVES - NONDESTRUCTIVE EVALUATION BY OPTICAL MICROSCOPY SAMPLE NO. Sample number s PSIV 20, 21, 22, 24, 25, 26, 27, 28 and controls wer e received for examination by optical microscopy. The components of the valve in each sample set were pho togr aphed prior to examination (Figur es 1-3) . METHODS All samples were examined under zeiss Univer sal stereo widefield optical micr oscope , equipped with indir ect reflected light. Magnifications from 7.9X - 24.6X wer e used. Micr ogr aphs are pr esented in Figur es 4-14. RESULTS Energized Elastomer Seat (Figures 4-5) The con tr ol energized elastomer seat is smooth and uniform. There 4a). are no indentations or impr essions on the sur face (Figur e The "used" ener gized seats have a deep "doughnut indentation in the cen ter (Figur es 4b & c, & 5). The shaped" rubber sur f ace at the indentation is glassy in appear ance. A small bubble is located in the center area of samples MSIV 22 & MSIV 26 (Figs. 4b & Sb). De-energized Elastomer Seats (Figures 6 & 7) The control de-energized elastomer seat is relatively smooth and uniform (Figure 6a). The used de-ener gized elastomer seats also have doughnut shaped indentations in the center of the seat (Figures 6b & c, and 7). These indentations are not as severe as those on the energized 7528 Aubum Rood
- km 1000. Po mswe ONo 44077 216/357 3300
Page 2 - J. J. Grimm December 1, ^1987 $CGIC6. L N , seats. The rubber sur f aces of the used seats are rougher than the sur f ace of the control. O-Rings (Figur es 8-12) The control o-rings are rounded and smooth (Figur e 8) . The sur f aces of the used o-r ings have thr ee basic appear ances:
- 1. Flattened with little or no distor tions (Figs. lla & b) .
- 2. Flattened with distor tion of the o-rings' edges (Figs. 9a, 10a, 12b).
- 3. Flattened with major changes at the o-r ings' edges and center (Figs. 9b, 106, 12a & c).
One side of one o-ring in samples tG IV 22, MSIV 24, MSIV 27, MSIV 28 has major changes occur across the o-r ing. The edges are glassy in appearance and the center s ar e buckled and folded (Figur es 9b, 10b, 12a & c). The opposite sides of the same o-rings have only slight (Figures 9a, 10a, 12b). distor tions at the o-r ing s ' edge Flow Control Valves (Fig. 13) Inside the valves (MSIV 20, 21), a dark ring of deposits can be seen visually. Examination of these rings (Fig. 13) reveals the complement of a degraded o-r in g , such as that in Figur e 12c. The o-ring residue appear s to have adher ed to the br ass body of the valve. but it is less pr The edominan oppositet. side of the valve also has a deposit, ('j's4 ' //1..-h ;QQ. a
/ .
Kath'y A. Kr utyhI$lowa jsb Atts. File Nos. 8702086M - 8702095M Notebook Ref.: 20294-82 Reviewed By: (0bb% 'd
l
- a. 0.8X MSIV 20 ,
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IUCt! L '.' APPENDIX G Main Steam Isolation Valves - O-ring Destructive Evaluation by Scanning Electron Microscopy
1 o'
'TO:~ J..J. Grimm - CEI FROM: K. A..Krutyholowa
.DATE: January 7, 1988
SUBJECT:
MAIN STEAM ISOLATION VALVES.- O-RING DESTRUCTIVE EVALUATION BY SCANNING ELECTRON MICROSCOPY SAMPLES The surfaces and cross-sections of the o-rings in sample sets MSIV.. Control, -24, -26, -27, and -28 were examined by Scanning Electron Microscopy (SEM)-and Energy Dispersive X-ray (EDX) micro-analysis and Wavelength Dispersive X-ray (WDS) microanalysis. CLIENT REOUESTS
.l.- To document any morphological changes in the o-ring surface.
- 2. To record changes in elemental composition of the o-ring surface.
- 3. To record-any morphological or elemental changes in the cross-section of the o-ring.
METHODS Scanning electron micrographs were taken on the JEOL 35C SEM, equipped with a Tracor Northern energy dispersive x-ray spectro-scopy (EDS) detector and a wavelength dispersive x-ray spectroscopy (WDS) microprobe. Before examination, the surfaces were mounted on carbon stubs and carbon coated. The cross-sections were cut with a razor blade, mounted in a vice clamp holder, and carbon coated. Elements from Na (Z=ll) thru U (Z=92) can be detected by EDS. Carbon, nitrogen and oxygen can be detected by WDS. 7528 Auburn Rood . Box 1000 Po<nesville.ONo 44077 216/357-3300
Pcgo 2
;J. J.. Grimm January 7, 1988 H
Backscatter electron-imaging (BEI) was used on both the surface and cross-sections of the o-rings. In this technique, the contrast is dependent upon the average atomic number. The brighter areas reflect the presence of relatively heavier elements. For example, Zn will have a brighter image than Cu which will have a brighter image than Si. CONCLUSIONS
- 1. The o-rings from the failed main steam isolation valves have flattened and are more brittle than the nonfailed (MSIV26) or. control o-rings.
- 2. A significant quantity of copper has penetrated approximately 100-150 pm into the failed o-ring. A secondary, more porous layer has formed at the edge. Within this layer (A), a significant quantity of oxygen is present.
- 3. Within the failed o-rings, portions of the o-ring have attached to the brass valve body and pulled away from the main portion of the o-ring.
RESULTS I. SEM/EDS Evaluation of the 0-rino surface A. Morphology & EDS of MSIV Control
- 1. 0-ring Morphology (Figures 1 & 2)
The o-ring is rounded with a few deposits at the surface. These deposits contain primarily Ca and Zn and the deposits are scattered randomly across the o-ring surface (Figures lb & d BEI, Plots 2, 3& 4).
- 2. O-ring EDS (Plots 1-4)
All EDS data is summarized in Table I. Sulfur Ca and Zn are present in moderate quantities. Si, C1, K , and Fe are present in minor quantities. I B. Morphology & EDS of MSIV26
- 1. O-ring Morphology (Figures 5 & 6)
The o-ring is still rounded. The inside edge has numerous score marks and has a flattened area l (Figure 5).
PageL3-J. J.-Grimm January 7, 1988 , Backscatter electron images of the o-ring surface indicate minor quantities of relatively heavier elements.such as Cu scattered randomly.
- 2. O-ring EDS (Plots 9 & 10)
All EDS data is summarized in Table I. Elements which include Al, Si, S, K,-Ca, Fe, Cu, and Zn are present in minor amounts on the o-ring surface. Near the inside edge of the o-ring, spot mode-analysis of the particles identify these as primarily Cu (Figure 6d, Plot 10). i C. Morphology & EDS of MSIV24, 27, & 28 O-rings from
- ' Failed Valve
- 1. 0-ring Morphology (Figures 3, 4, 7, 8, 9& 10)
The o-ring has flattened; the surface appears to
.have been attac hed and peeled of f. Backscatter electron images of the o-ring surface indicates i
large quantities of heavier elements such as Cu-and Zn cover the surface.
- 2. 0-rings EDS (Plots 5-8, 11-17)
All EDS data is summarized in Table I. Cu & Zn . are present in major quantities. When comparing the copper counts in the three failed samples to the control, the copper counts are significantly higher in the failed samples. Conversely, the Ca counts are significantly lower in the failed samples in comparison to the control. i In sample MSIV24, moderate quantities of Si & S and minor quantities of A1, Ca, Fe, Ni & Pb are present. Plots 6, 7& 8 are the result of spot mode analyses of individual areas a, b& c in Figure 4b. In sample MSIV27, moderate quantities of Si and minor quantities of S, Cl, Ca, Fe, & Pb are present. Plots 12 & 13 are the result of spot mode analyses of individual areas b & d in Figure 8b. In sample MSIV28, moderate quantities of Si, S& i Pb and minor quantities of Ti & Al are present. Plots 15, 16 & 17 are the result of spot mode analyses of individual areas a, b & c in Figures 9 & 10. Lead (Pb) appears to have concentrated in specific areas as shown in Figure 10c and Plot 17.
Pcge 4 J. J. Grimm January 7, 1988 II. SEM/EDX Evaluation of the O-rina Cross-sections A. Morphology & EDS of MSIV Control (Figures 11 & 12) ?
- 1. Morphology The cross-section is very uniform from the edge to the center of the o-ring. No morphological differences are noted in the control.
- 2. 0-ring EDS/WDS Plots 18 & 19 The EDS/WDS data are located in Table II. No elemental differences were noted between areas A and B (Figure 13c) in the control. Both areas had a major quantity of C, S& Ca and a minor quantity of Si, Cu & Zn.
Backscatter electron images of the cross-section only revealed a uniform distribution of relatively heavier elements such as Ca and Zn. B. Morpholgoy & EDS of MSIV26
- 1. Morphology (Figures 15 & 16)
The cross-section is very uniform from the edge to the center of the o-ring. No morphological differences are present across the sample. The morphology is similar to the control.
- 2. EDS/WDS O-ring Cross-section (Plots 22-23)
The EDS/WDS data are located in Table II. No elemental differences were noted between areas A
& B (Figure 15c). Both areas had major quantities of C, Si & S, and minor quantities of Ca, Zn & C1.
The number of Cu counts is significantly higher in sample MSIV26 than in the control. The Ca counts are significantly lower than in the control. C. Morphology & EDS of MSIV24, 27 & 28 Cross-section of 0-rings from Failed Valve
- 1. Morphology (Figures 13 & 14, 17-20)
The cross-section reveals two distinct areas, A and B (Figures 13c, 17c & 19c). Area A is approximately 100-150 pm deep at the edge of the o-ring. Area A is much rougher and appears to be more porous.
Pago 5 J. J. Grimm January 7,'1988 Samples MSIV24 & MSIV28 have 2 sides of the flattened o-ring containing_ area A. Sample MSIV27 has 3 sides
.of the flattened o-ring containing area A.
- 2. EDS O-ring Cross-section (Plots 20-21, 24-27)
The EDS data is located in Table II. There is a significant increase in copper counts when ec= paring the three failed samples to the control. In additien, area A in the three failed samples has a larger number of copper counts than in Area B. The si ccunts have increased significantly and the Ca counts have decreased compared to the control. In sample MSIV28, there is a significant quantity of oxygen present. Relatively no oxygen was present in sample MSIV26 or in the control. b4 ' Kathy A. Krutyholewa jsb Atts. File No.: 8702086, 8702091 8702094, 8702095 Notebock Ref.: 20294-88 Reviewed By: M @ btN% e
c Table I O-ring Surface Energy Dispersive X-ray (EDS) Microanalysis Net Counts per Second 100X Area Si S Ca Cu Zn Control (Plot 1) 18 60 65 20 83 MSIV24 (Plot 5) 52 26 6 '256 117 MSIV26 (Plot 9) 19 11 3 31 14 MSIV27 (Plot 11) 55 27 3 333 154 MSIV28 (Plot 14) 30 20 2 241 115
Table II Cross-sections of 0-ring Ercrgy Dispersive X-ray (EDS) Microanalysis Wavelength Dispersive X-ray (WDS) Microanalysis Net Counts per Second 2000X Area Control C N O Si S Ca Cu Zn Area A (Figure lle) 5,057 0 0 11 118 91 26 47 Area B (Figure 11c) 4,896 0 7 10 111 76 24 49 MSIV24 Area A (Figure 13c) NA NA NA 89 74 7 97 48 Area B (Figure 13c) NA NA NA 70 78 6 66 27 MSIV26 Area A (Figure 15c) 4,381 0 0 103 89 5 66 25 Area B (Figure 15c) 3,834 0 0 91 87 9 64 25 MSIV27 Area A (Figure 17c) NA NA NA 186 66 5 124 58 Area B (Figure 17c) NA NA NA 95 97 7 40 12 MSIV28 Area A (Figure 19c) 4,584 0 281 177 77 5 159 84 Area B (Figure 19c) 4,576 0 52 89 82 3 42 14 NA = Not analyzed
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Plot 1 i MSIV Control l O-ring Surface ! 100X Arca l li ll ! !I l l!I ll t !! Il l! I ll t !I l l I !I ll t !I ll l !I l l t !!Il l !! il l! I ll t !! Il l!! Il l!I ll i! I ll t !I l l 1lI ll t !! H i! I l ub 83
. KAK LISTiriG w EflERGY AREA EL. (dC L!!;E
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.m MSIV Control 0-ring Surface l Spot Mode A; Fig. 2b n
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,,, - 1 1.818 1614 2N LA
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t' 10 C J l MSIV Control O-ring Surface Spot Mode B; Figo 2b
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r elon 4 MSIV Control O-ring Surface Spot Mode C; Figo 2c lt1itltIit!nn!nnl:ntlnnl:nt! tut l:ntl1nt!nn!tn1lnn!nn!nn!nn!1nt!nubudun[U PEAK LIST!f4G 9 DiERGY AREA EL. 4 0 LINE u- 1 1.758 2825 SI m - 2 2.318 !!d83 S m
.o F j; y q 3 2.651 448 CL m O x . o 4 3.295 1321 K m M o O 5 3.690 18941 CA m 1 4 4.823 2 _
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?o - N M r n o r- ors a e, - es m r n o es (o e o W - - - - - - - - - - N L
riot > MSIV24 O-ring Surface 100X Area
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Plot 6 MSIV24 O-ring Surface Spot Mode A; Fig. 4b E,; l111!!!III!I11 t l t III!!11 t l111I!t iI!!!11I"It s !! t t II!!II t !!11 t!I11!!!Ii1ll1II! 11 tl111 tllIt ll11 t I! t t t t !Il n y PEAK LISTING DERGY AREA EL. #1D LIFE _ 1 0.982 1221 ZN LA _ p y , 2 1.747 1811 St M O M
^
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- - - - - - - - - - N
Plot 7 MSIV24 0-ring Surface Spot Mode B; Fig. 4b ltiti!niti!s til!Iiti!it ti!ilit!!It t!!Itt!Ilit!!Ill!Illt! fill!!Ill!!!!!!!If f!!!!flfillillflif filillifill PEAK LISTING
? ENERGY AltfA EL. 410 LINE l E -
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Plot 8 ! MSIV24 0-ring Surface Spot Mode C; Fig. 4b n' 1111 till1111l11111111till till 1111 ((t 1111 till 1111 1111 1111 till Illl 1111 Illt illI llI 8, PEAK LISTING v,
~
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'8 10 8.931 1979 CU N8 F _
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l Plot 9 l MSIV26 0-ring Surface 100X Area l ttit lt t t tlt t t t! tit tlt t t tlt tit!t it t!t it t! tit t lt t t t!t it t! tit t! tit tl tit l{t til! tit t ! tit tlt t t tlt t t tlt t t tlti
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PEAK LIS1114 nt DIERGY AREA EL. 6600 LitIE
! 8.934
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Plot 10 MSIV26 l O-ring Surfaco l Spot Mode A; Fig. 6b
~Z e
j.- li n i i n n i n n i n n i n n i n n i n n i n ntifi l u u l o n i n n l u n l u n l n n i n n i n n i n n i n n l o n l u 8, PEAK LISTits d* MM AREA EL. Mm LINE n' I 8.938 444 CU IA 2 1.483 1839 AL M F >
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7 8.918 4858 CU N8
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Plot 11 MSIV27 O-ring Surface 100X Area
-r
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, PEAK LIST!f4G DERGY AREA EL. 440 Lit 4E
([,, ! 8.999 1324 34LA 2 1.462 442 AL G - p -> l2 - 3 1.745 8628 51 M g !j { 4 2.325 4123 S M J o
" 5 2.650 512 CL M d 3.473 989 CA M 7 6.393 481 FE M o
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Plot 12 MSIV27 O-ring Surface _ Spot Mode B; Pig. 8b l H H lIlI t lt Ii1lIII t lIIII!III t !!1I I!I H i n t l H H ! n n ! n H l H H ! H H ! H H ! ! H I l H H ! n t dub 1uU}D
3 PfAK LISTING k
ETUGY AREA EL. 6440 Litti -
*<=_ 1 8.978 1248 CU LA OR 2N LA?
E U 3D 2 1.748 1895 SI E
- 4 Q 3 2.355 933 S u d o o 4 4.375 568 FE u E 2 _
5 8.030 37005 CU M - J y 4 8.d15 16412 be u 7 g,93, 193 CU MS i.il .o u 8 9.555 2354 2N M8 F PJ _ Z - O hl %
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_ . . _ . ._ _ _ _ . _ _ _ _ _. . _ _ _ _ _ _ . _ _ _ _ _. __ _ _ _ _ __ _ . ~ ___ _ MSIV27 O-ring Surface Spot Mode D; Fig. 8b I In n i n n in n in nin nli n ilu nin ni n nin ni n nin nin ni n nin n in nin nli n ii n n innlu
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..$ PEAK LISilNG tt DERGY AREA EL. M L!r(
I t.982 378 ZN LA F! > F 2 1.448 1479 AL M C $5 3 1.747 12179 51 M J , 3 4 2.315 9449 $ m i n 5 2.455 539 CL M 9 - d 3.477 917 CA M
- 7 S.038 4491 C!l M J
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riot 14 MSIV28 0-ring Surface l 100X Area ,
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v. nL PEM LIST!!E
, ENERGY AliEA EL. (de LINE p l -, *-) 1 1.000 821 2N LA O y 3 2 1.473 414 AL u j o 3 1.743 4652 51 M o
g .9 4 2.324 3449 S M ' o 5 4.587 85411 M - 3 o 4 8.02d 25294 CU M q
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to m _ 9 9.552 1742 2N M8 U o d NJ
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rsot n MSIV28 0-ring Surface Spot Mode A; Pig. 9a 3 l1111!!t11!!fil!!11I!!I11!!111!I11I!!111 1111 ! t 111!! 111!I 11 !!Ill Ib t !! t t I!! !! !!! 11 !!! 11 t !! fit !! 111 !!1
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PEM LISTitiG SL DiERGY AGEA EL. f4i0 LinE I 8.982
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- APPENDIX H Main Steam Isolation Valves - Energized Elastomer ' Seats
- Destructive Evaluation by Scanning Electron Microscopy -
t .i r d f 4 l l h f y ., - - - , -, 2----.- ,w,---,.-r. _ r..--r-e-- -- --
TO: -J. J. Grimm - CEI
'FROM:- K..A. Krutyholowa DATE:- January 11, 1988
SUBJECT:
MAIN STEAM. ISOLATION VALVES - ENERGIZED ELASTOMER SEATS - DESTRUCTIVE EVALUATION BY SCANNING ELECTRON MICROSCOPY
' SAMPLE NO.
The surfaces &. cross-sections of energized elastomer seats from samples MSIV Control, MSIV24, MSIV26 and MSIV27 were evaluated by scanning electron microscopy (SEM) and energy dispersive x-ray (EDS) microanalysis. The cross-sections were also examined by optical microscopy (OM). The center cones of the flow control valves (MSIV20 & MSIV21) were' evaluated oy optical microscopy. CLIENT REOUEST
- 1. To determine the depth of the indentation present in the failed and not failed energized elastomer seats.
- 2. To document any morphological or elemental changes in the energized elastomer seats.
- 3. To record any morphological or elemental changes in the cross-section of the energized elastomer seats.
METHODS Optical microscopy was done under the Zeiss stereo widefield optical microscope (SV-8) equipped with indirect reflected light. Scanning electron micrographs were taken on the JEOL 35C SEM, equipped with a Tracor Northern Energy Dispersive X-ray Spectro-scopy (EDS) detector. Before examination, the surfaces were mounted on carbon stubs and carbon coated. After the surfaces were examined by SEM/EDS, the cross-sections of the seats were prepared. The cross-sections were cut with a razor blade exposing the indented area of the seats. They were mounted onto carbon stubs and carbon coated. 7528 Auburn Rood Box 1000. Poinesvino. Ohio M077 216/357 3300
S
.Pago 2 J. Grimm.
'J.
January ll, 1988'
.c-Elements from-Na (Z=ll) thru LF(Z=92). can be detected by EDS.
' Backscatter. electron imaging.(BEI)'was used on both.the surface-3 and. cross-sections of.the energized elastomer seats (EES).(In b this' technique, the1 contrast is dependent upon the-average atomic number.- ;The brighter areas reflect the presence of relatively heavier elements.- For example, Zn'will.have a brighter. image-than Cu'which will have'a brighter image than Si.
CONCLUSIONS-
- 1. The failed energized. elastomer seats have an indentation which is' deeper than the "not failed" seat.
'2. No morphological changes have occurred to the rubber beneath the indented areas.
- 3. More particles have deposited within the-indentations'of the failed seats versue the "not failed" seats.
- 4. More copper is present at the surface of the indentation of the failed seats than in the not failed and control seats.
RESULTS I. Energized Elastomer Seats - Surface A. Morphology & EDS - MSIV Control
- 1. Morphology (Figure 1)
The MSIV Control energized elastomer seat is level with no indentation. Particles of material are visible making the surface relatively rough.
- 2. EDS (Plot 1)
All EDS data is summarized in Table I. Major quantities of S & Zn and minor quantities of Si, C1, Ca , K, Fe and Cu are present in the rubber. B. Morphology & EDS - MSIV26 - Not Failed
- 1. Morphology (Figures 4 & 5)
The MSIV26 energized elastomer seat has an indentation ring at the center. Within this indented area, there are small quantities of particles (Figures 4b, Sa).
Page'.3 J. J. Grimm January 11,11988
- 2. .EDS (Plo't's 5,.6 & 7)
All EDS data is summarized in Table I. In the indented area A, major quantities of Si,&-Zn and minor quantities of Fe, Cu, S,-Cl and Ca are present.
-Area B in Figure 4a has less Cu present than in area A.- Arda C'in Figure 4a has less Cu and signi-ficantly more.Fe than in area A.
C. Morphology & EDS - MSIV24 & 27 - Failed
- 1. Morphology (Figures 2, 3, 6, 7)
The MSIV24 and 27 energized elastomer seats have an indentation ring at the center. Within these indented areas are large quantities of particles (3a & b, 7a & b).
- 2. EDS (Plots 2-4, 8-10)
All EDS data is summarized in Table I. : In the: indented area A.(Figures 2a & 6c), major quantities of Si, Zn & Cu, moderate quantities of S& Fe, and minor quantities of Cl, Ca & K are present. Examination of the seats by backscatter' electron imagina (Figures 2b & 6d) _ reveals numerous bright particles in the indented area A. This~ indicates the presence of heavier elements such as Cu & Zn. 4 Area B in Figures 2a & 6c have less Cu than in area. - A. Area C in Figures 2a & 6c have less Cu and significantly more Fe than in~' area A. II. Energized Elastomer Seats - Cross-sections. A. Optical Micrographs - Cross-sections (Figure 8) The cross-sections of the energized elastomer seats revealed the depth of the indentations for the four samples (MSIV Control, -24, -26 & -27). They were as follows: MSIV Control - O pm 4 MSIV24 350 pm MSIV26 230 pm MSIV27 350 pm
- - , - - -- -- ., . . _ . ,- , - . ., . .,m _ , . _ _ , . , _ , , -,.,,.,p, m
c Page 4 J..J. Grimm January 11,' 1988
'The'two failed energized elastomer. seats had a deeper
. indentation than the "not failed" energized-elastomer t seat MSIV26..
.B. Morphology'& EDS - MSIV Control (Figure 9)
The. cross-section of the control seat reveals a uniform morphology. The backscatter electron image reveals a uniform distribution of brighter particles. EDS data is located in Table II. Major quantities of Zn & S and minor quantities of Si, Cl, K , Ca, Fe 6 Cu were present in areas A & B (Figure 9a) of the cross-section (Plots 11 & 12). C. Morphology & EDS - MSIV26 - Not Failed
- 1. ' Morphology(Figures 12 6 13)
When examining the area directly beneath the indented area AL(Figures 12a & c), no changes have occured to the ruboer.
- 2. EDS (Plots 15 & If EDS data is loce hble II.1 Major quantities of Si, Zn & S ant ....nor quantities of Cl, Ca, Fe
& Cu were found in area A, Figure 12a. Backscatter electrcn imaging of the cross-section of seat MSIV26 identified very few particles within the indentation 1 (Figures 12b, d& 13b).
D. Morphology.& EDS - MSIV24 & 27 - Failed
- 1. Morphology (Figures 10 & 11, 14)
When examining the area directly beneath the indentation, no morphological changes have occured (Figures 10 $ 14). Numerous particles and debris can be found in the indentation.
- 2. EDS (Plots 13, 14, 17 & 18)
EDS data is located in Thble II. Major quantities of Si, Zn & S, moderate quantities of Cu and minor quantities of Cl, Ca & Fe were found in area A. uw - v- ,. - -y-.,, .- . , , .- -,---,3-y,--., , ,, , , ~ - -
4 Pago 5 Ji J. Grimm January 11, 1988 Backscatter electron imaging of the cross-section of seats MSIV24 & 27 identified numerous particles within the indentation (Figures 10b & d, 14b & d). These particles have large amounts of Cu, Zn & Fe. E. Optical micrographs - cones from flow control valves Figures 15a & b, and 16a & b have. areas.(arrows) where pieces of material appear to have adhered to the lip of the cone. bh Kathy A. W f t$N r Krutyholowa jsb Atts. File No's, 8702091, 8702006, 8702093, 8702094 Notebook
Reference:
20294-93 Reviewed By: LO R bgk
A Table I 1 Energized Elastomer Seats - Surfaces Energy Dispersive X-ray (EDS) Microanalysis Net Counts per Second 400X Area-Si S- Cl Ca Cr Fe Cu- -Zn ~ Pb MSIV-Control 28 59 16 11 0 7 10. 199 0 (Figure la) MSIV24 (Fig. 2a) . Area A 255 44 5 6 2 57 87 166 2 Area B 123 56 15 6 1 56 13 180 0 Area C 163 54 13 4 0 85 11 172 0 MSIV26 (Fig. 4a) Area A 210 40 11 4 1 41 40 163' 1 Area B 190 48 19 4 2 42 12 142 - l~ Area C 130 51 12 7 2 73 7 133 /0-MSIV27 (Fig. 6c) Area A 172 35 12 5 4 82 55 218 .1 Area B 175 48 13 5 1 63 13 137 0 Area C 181 51 19 9 1 85 '9 146 1 i* u _ ,
Ta'le o II Energized Elastomer Seats - Cross-sections Energy Disporsive X-ray (EDS) Microanalysis Net Counts per Second 3000X Area Cu Si S Cl Ca Fe Zn MSIV-Control (Figures 9a) A 34 91 6 9 6 8 162 B 17 86 2 5 3 4 155 MSIV24 (Fig. 10a) A 111 97 3 5 11 14 120 B 1 14 i 15 4 6 197 MSIV26 (Fig. 12a) A 80 83 2 4 6 9 113 B 1 14 1 5 1 6 173 MSIV27 (Fig. 14a) A 212 70 6 11 53 32 100 B 3 22 0 6 6 10 171
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,4 ,
[ ' e- $ .. . - MSIV24
~
[, Energized Elastomer Seats l 7~ e. <g.; . .
- Q - 4
- / t . ,.- / ~ f 'z -g , ,g*;,ek Failed
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' '. " r ;f,. ,' t, <
, ;". t. ' MSIV26
- . J..,-
t ,.'15.*. 's , f+ %y J Energized Elastomer Seats
, . ' .. ,,- . Not Failed
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d' Surface
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C=Outside 25KU. 46.
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, .- MSIV26 f
Energized Elastomer Seat Not Failed
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l MSIV27 En zed Elasterer Seat Surface
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Plot 2 MSIV24 Energiged Elastomer Seat Surface - Failed Area A = Indent
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Plot 3 MSIU24 Energized Elastomer Seat Surface - Failed Area B = Center l 1111 ! ! l l l !! 11 l l 111 l l 1111 ! I 111 ! ! 111 ! ! 111 ! I 111 ! ! 111 l l 111 ! ! ! ! ! ! ! 1 I 1 l I l l ! ! I l l l ! I l l l ! ! I l l ! I l l l ! ! I I I ! ! 111 ! ! 1
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Plot 4 MS1V24 Energized Elastomer Seat Surface - Failed Area C = Outside
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Plot 8 MSIV27 Energized Elastomer Seat Surface - Failed Area A = Indent
-s
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Plot 9 MSIV27 Energized Elastomer Seat ' Surface - Failed Area B = Center e ! !! ! ! !! I l l!I l l l !I ll i ! ! ! ! !!I l l t ! ! Il l ! I l l t ! f i l l !! I l l ! ! I t !! I I l l ! ! I l l ! ! I l l ! ! 111 ! ! 1 f 1 ! ! 11 lll 111! ! 111 1111)1J
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Plot 10 MSIV27 Energized Elastomer Seat Surface - Failed Area C = Outside
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Plot 11 MSIV Control Energized Elastomer Seat Cross-section Area A - Figure 9a
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Plot 12 MSIV Control Energized Elastomer Seat Cross-section Area B - Figure 9a
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Plot 13 MSIV24 ( Energized Elastomer Seat Cross-section - Pailed Area A - Figure 10a l
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Plot 14 MSIV24 Energiged Elastoaer Seat Cross-section - Pailed Area B - Pigure 10a
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Plot 15 MSIV26 Energized Elastomer Seat Cross-section Area A - Figure- 12a Not Failed r bi!!!!!!Ull 1111 filfilll! '' III' Il'i I 't' ltlfl t1t fit f fi f f1filtf tlflhffll' fl n.
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Plot 16 MSIV26 Energized Elastomer Seat Cross-section - Not Failed Area B - Figure 12a r
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Plot 17 MSIV27 Energized Elastomer Seat Cross-section - Failed Area A - Figure 14a lll11!111 !I111!I111ll11ll1 lit!!Ill!illf!!!ti!Ilf t!Illi!!Ill!titi!!Ill!llit!!III!!!It!ttit!illi!!I1!!!I
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Ricer ce. i APPENDIX I Infrared Examinations of O-rings from MSIV Units I
r TO: John Gr imm - CEI FROM: J. M. Sander s DATE: January 15, 1988
SUBJECT:
INFRARED EXAMINATIONS OF O-RINGS FROM MSIV UNITS INTRODUCTION The purpose of this infrared study of the o-rings is to determine if this technique can detect possible chemical change in th e o-ring ma ter ial (EPDM) after usage. If such a change could be detected and identified, it is believed that the information would also apply to the valve seats since they are also composed of the same mater ial and exposed to the same environment. Thus, it is feasible that an infrared study of the o-rings may lead to the cause of f ailur e for some of the MSIV's in the fast close test. EXPERIMINTAL Infrared spec tr a wer e obtained with a Nicolet 7199_yFT-IR spectrometer which was operated at a resolution of 4 cm . A Barnes Model 300 ATR unit was used with both KRS-5 and germanigm cr ys tals. The angle of incidence was set to either 30 or 45 . The ATR is a sur f ace technique with an average depth of penetration of approximately 10 p m. In an ef for t to obtain good quality spectr a from the o-r ing s , some experimentation was necessary with some of the parameter s used in the ATR technique. Infrared spectr a wer e obtained from o-rings utilizing bo th germanium and KRS-5 crystals and for this wor k , the KRS-5 appear ed to provide better results. Different angles (30 & 45 ) of incidence were also used with the crystals but did not produce any significant dif fer ence in the results. The most impor tan t f actor s appeared to be the placement (position) of the o-ring segments on the erystals and the pressure used to hold them against the cr ys tal. It was not possible to reproduce these par ameter s and repeats wer e made as necessary to obtain good spectra. Ef for ts wer e also made to grind a por tion of the o-rings in order to utilize the KBr technique; however, the results from these ef for ts wer e questionable and it was abandoned. 7528 Aubum Rood
- Boa 1000
- Po.nesMe.ONo 4077 216/357 3300
/.
.k ' Page 2 N O K E E' J. J. Grimm Januar y 15, 1988 RESULTS The fir st set (N-6968-74) of spec tr a represent those obtained during the experimental stage of this investigation. In general, these spec tr a , except the KBr ones, are of f airly good quality but do r epr esen t some effects fr om var ying parameters as discussed above. For this reason, there may be some dif fer ences when compar ing these spectra to similar ones acquired at a later per iod. However, such dif ferences are not ar tif acts but result from the in f r ar ad beam "seeing" a somewhat different overall por tion of the sample due to a second sampling and the inhomogeneity of the used o-ring. A second set (N-6980-88) contains spec tr a from all the o-r ings and was obtained under similar conditions. In comparing these spec tr a , the most significant observation seems to be ge formation of two str ong infrared bands near 1530 and 1425 cm . This does not occur in all the spectr a but is most apparent in the spectr a from the MSIV22, 24, and 28 o-rings. These bands strongly suggest the presence of a car boxylic acid salt. The bands (1530 & 1425 cm y) ar e very characteristic of car boxylic acid salts and their positions are fairly constant regardless of the type of salt (i.e. Na, Ca, Mg, 2n, e tc. ) The most likely possibility would be zine stearate since bo th zine oxide and s tear ic acid ar e used in many EPDM for mula tion s . In addition, many of the spectr a show evidence for the pr esence of silicone oil (lubr ican t) og the o-rings by showing infrared bands at 1252, 1025, and 800 cm . The following list provides a summary of the information obtained from the spectra of the o-rings. 0-r ing Spectr a Comments MSIV22 N-6982 Alkyl acid salt, silicone oil MSIV24 N-6986 Alkyl acid salt, silicone oil MSIV25 N-6981 Alkyl acid salt, silicone oil MSIV26 N-6980 Spectrum fairly similar to control MSIV27 N-6987 Spectrum fairly Pimilar to control MSIV2B N-6988 Alkyl acid sal'.;, silicone oil
i _ swL e*e. Page 3 Ricerca. i J. J. Grimm Januar y 15, 1988 Although the alkyl acid salt and silicone oil were not detected on some rings, this does not indicate that these mater ials ar e absent in these cases but that they wer e not detected on the par ticular examination represented by the spectr um. However, it is fair to assume in such cases that, if pr esent, the materials would likely be at a low level compar ed to the ones which showed s tr ong evidence for the pr esence of the acid salt and silicone oil. In addition to the o-r ings, some of the black material from the area where the o-r ing had contacted the valve body was r emoved from FGIV20 & 21 for in fr ar ed examination. This ma ter ial was ground and the IGr technique was used to obtain spectr a (N-6999 & N-7000). These spectr a wer e very similar and like some of the a bo ve , strongly suggest the pr e sence of an alkyl acid salt and silicone oil. CONCLUSIONS The in fr ar ed examinations suggest that none of the o-r ings have under gone severe oxidation since none of the spectra show the presence of a s tr ong car bonyl band. However, as indicated previously, many cf the in'r ar ed spectra do show the pr esence of car boxyla te bands. Suca bands could pssibly result fr om oxidation but, in these cases, are strongly believed to be due to the presence of a compound formed in the EPDM formulation. Many EPDM formulations contain Zno and stearic acid which react to form zine stearate dur ing the cur e of the rubber. The zine s te ar a te can and is known to migr ate to the sur f ace ( ' bloom' ) of EPDM r ubber s and this pr oce s s would be accelerated with the addition of heat. As a result, it seems very likely and highly probable that the alkyl acid salt on the sur f ace of some of the o-r ings or iginated from the EPDM, It was not possible to per form an infrared examination of the valve seats because of their small size and unique shape. However, it seems reasonable to assume that some of the valve seats also have an alkyl acid salt on their sur f aces since they ar e also composed of EPDM and ar e also in close pr oximi ty to the o-rings. If this is the case, the following rationalization may explain the cause or reason why some of the values failed the fast close test. The pr esence of an alkyl acid salt such as copper stearate or zine stearate on the sur f ace of the valve seat could act as a glue if the 1
Page 4 _ J. J. Grimm J anuar y 15, 1988 Riccut. - temperature of the valve exceeded s260 F. The reason for tpis is thag copper and zine stearates have melting points of 257 F and 266 F, r espectively. Thus, at these temperatures, the alkyl acid salt would liquefy and could ' wet' the brass outlet por t seat in contact with EPDM. If the temperature elevation was an isolated event, the alkyl acid salt would solidify on cooling and could act as a glue te; r e tar d or pr ohibit the opening of the valves. While it's not possible to prove this theory, it could be tested by ensur ing that the valves never exceeded a temper a tur e of N240 C.
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