Analysis of Alloy 22 Weight Loss due to General Corrosion

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Analysis of Alloy 22 Weight Loss due to General Corrosion

3-5-2008

Yucca Mountain Project

LSN Relevant

Sandia is a multiprogram laboratory operated by Sandia Corporation a Lockheed Martin Company Sandia for the United States Department of Energys National Nuclear Security Administration Nationalr Laboratonesunder contract DE-AC04-94AL85000 ~

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Background Introduction

bull The corrosion rate used in the TSPA-LA is based on corrosion test data from 5 year test specimens and generated in -FY01

The 95 year test specimens are being readied to provide new data that would presumably validate the TSPA-LA corrosion rate

bull In a technical review of the 5 year data and a review of the methodology a vulnerability was uncovered

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Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28middotFeb-2008 OCRWM Lead Lahoratory for Repostory Systl1tlS

2

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Issue Summary bull There are documented repeated and potentially significant

excursions from the ASTM standard for corrosion test specimens bull The cleaning of 5 year corrosion coupons from the LTCTF may have

been incomplete leaving samples in an indeterminate state bull Complete cleaning of the 5 year coupons could result in larger weight

loss values than are currently used for the general corrosion model bull Complete cleaning of 95 year coupons might show an increase in

corrosion rate compared to the existing 5-year data bull While corroborative data exist in the literature almost all corrosion

studies reviewed to date reported corrosion rates greater than the 5 year data from the LTCTF

bull Net Effect - Our TSPA-LA corrosion rate may not be conservative and if not could

significantly affect the results for the EIS and the peak dose results - Basic defensibility of the TSPA-LA corrosion rate is jeopardized without

some confirmation in essence the rate we now use is an assertion - A CR will be initiated

Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28middotFeb-2008 OCRWM Lead Lahoratory for ReposItory Systems

3

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Path Forward

bull Initiate a CR

bull Corrective Action Initiate and accelerate new scope to collect the data that will confirm or refute the conservatism in the TSPA-LA corrosion rate before docketing

bull Regenerate and re-evaluate the 5 year data and generate 95 year data correctly

- ROM estimate is -650K refined estimate pending

bull Expert judgment is lt50 chance the TSPA-LA rate is invalid but given the critical nature of this parameter is must be confirmed

bull Prevent Recurrence Transition the corrosion test samples testing and data generation to a fully ASTM compliant methodology with qualified technicians and equipment

bull Conclusion Does not effect going forward with the LA if we generate the confirmatory data prior to docketing

Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28-Feb-2008 OCRWM Lead Lahtgtratory for Rf1positcry Systems

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The cleaning procedure used on the 5 year samples does not appear to meet the intent of the ASTM guidelines ASTM G1-90 Standard Practice for Preparing Cleaning and Evaluating Corrosion Test Specimens (reapproved 1999)

ASTM G1-90 TIP-CM-51Lab notebooks (Pre-exposure) 631 Degrease in organic solvent or hot alkaline cleaner 632 Pickle in an appropriate solution if oxides or tarnish are present

Samples in the LTCTF were tested in the asshyreceived condition from the supplier (Notebook 241 p16) or samples were degreased in acetone (McCright 1998 [DIRS 114637] p22-11)

(Post-exposure) 711 By weighing the control specimen before and after cleaning the extent of metal loss resulting from cleaning can be utilized to correct the corrosion mass loss

TIP-CM-51 Appendix A Weight loss on control foil samples was shown to be on the order of 01 mg (resolution of balance) No data from Alloy 22 coupons was located No corrections made to weight loss data

(Suggested practice) 7121 The cleaning procedure should be repeated on specimens several times

TIP-CM-51 7231 If the weight is at or below the initial starting weight cease cleaning the specimen and proceed to step 725 below

(Suggested practice) 7122 The mass loss should be graphed as a function of the number of equal cleaning cycles the mass loss due to corrosion will correspond approximately to point B [see graph next slide]

TIP-CM-51 725 Selected specimens will be checked by scanning electron microscopy (SEM) to ensure that all the corrosion products are removed If corrosion products remain on the specimen repeat cleaning procedure

iilIl Sandia National Laboratorle Analysis of Alloy 22 Weight Loss due to General Corrosion 28middotFeb-2008 OCRWM Lead Laboratory for postory Systems

6

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ASTM guidelines previous control samples and recent scoping tests suggest that the weight loss per cycle should be negligible on

Wight Los cn Ccntrol Samples for th Hel CIanlna Processa thoroughly cleaned sample OOO1-a 1I j i-~~l ~~ O~)14 Ji -_OCA287~~~

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Number of Cleaning Cycles weight Change From Cycle N-1 to Cycle N for Hel Cleaned AllOY 22 samples

ASTM G1-90 7122 the mass loss due to 000120

corrosion will correspond approximately to point B ---OCA8S ___OCA2Eiasect 000100

Foil Weight Loss (g)

DFA01 00000

DFA02 00001

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TIP-CM-51 Appendix A foil samples (controls) Cycl4f umber N

exposed for 3 min in HCI bath Feb 08 Scoping tests Alloy 22 coupons in HCI bath

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Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28-Feb-2008 OCRWM Lead Laboratory for Rfpasitorj Systems

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With Low Weight Losses Technique and Equipment Sensitivity and Precision are Vital

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ASTM G1-90 7122 the mass loss due to corrosion will correspond approximately to point B

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Cycle Number

In practice much care must be taken to perform the cleaning properly to obtain meaningful results Blue and Red curves represent different cleaning techniques on identical blank samples

Sandia National Laboratories Analysis ofAlloy 22 Weight Loss due to General Corrosion 28middotFeb-2008 OCRWM Lead Lnhnratory for Repostory Systenll

8

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The process used to clean the 5 year weight loss samples likely left the samples in an indeterminate state

Weight Change for 5-Year Alloy 22 Weight (A) Approximate weight change from Loss Samples

control experiments in TIP-CM-51 00020

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IlttlP bull All 5year Ailoy 22 Welgbt-Loss SlIllple$

Appendix A (8) Approximate cycle to cycle weight

change from scoping tests Feb-DB (for cycles 4 and 5)

Weight Change From Cyde N-1 to Cycle N for 5-Year Alloy 22 Weight Loss Samples

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Corrosion rate corresponding to 00005 g weight loss 00 ~ r I II I I on 5 year coupons - this mass loss was often exceeded

4 G 8 10 12 142 in a single cleaning cycle -Genofol Conoltion _ (nnrye)

Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28-Feb-2008 OCRWM L~ad Lahora1ory for RepOSitory Syslems

9

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The process used to clean the 5year crevice samples likely left the samples in an indeterminate state

(A) Approximate weight change from control experiments in TIP-CM-51 Appendix A

Weight Change for 5-Year Alloy 22 Crevice Samples

(8) Approximate cycle to cycle weight change from scoping tests Feb-08 (for cycles 4 and 5) i ~~~~ t ~~ ==-- ~~----~~=

poundc 0006 L----- Weight Change From Cycle N-1 to Cycle N for 5-Year Alloy 22 Crevice Samples

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Cleaning Cycle Number ~~ 0004 bull I ICOF -All 5-year Alloy 22 Crevice samples ~i -----1--------------- shy0002

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025 Corrosion rate corresponding to 0001 g weight loss on 5 year coupons - this mass loss was often exceeded in a single cleaning cycle - shy

5 10 15 20 25

General Corrosion Rate Inor)

Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28middotFeb-2008 OCRWM Lead Lahoratory for REpostOry Systems

10

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Complete cleaning of the 95 year Alloy 22 weight-loss samples may incorrectly indicate an increase in corrosion rate

Example 95 year exposure resulting in 12 mg of observed weight loss

(12 mg is the approximate weight loss observed on recently cleaned unexposed Alloy 22 coupons)

876xl09 middotO0012g 869g em3 bull 30em 2 bull 83220hrs = 485nm yr

equation taken from ANL-EBS-MD-000003 Rev 03 Eq 6-7 p6-27

ECDF - All S-year Alloy 22 Weight-loss Samples

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General Corrosion Rate (omyear)

Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28middotFeb-20oa OCRWM Lead Laboratory for Repository Systems

11

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Complete cleaning of the 95 year Alloy 22 crevice samples may have indeterminate results as no control data have been collected for samples with the crevice sample surface finish

loss coupons and one surface of crevice coupons

(B) Surface finish on one face of crevice samples

Images from L Wong (2004) [DIRS 174800] Figure 4 p15

-~----- (A) Typical mechanical polish for weight

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o Measured Data i ooosmiddot I I 000 8o I I

o 5 10 15 20 25 3025 General Corrosion Rate (nmlyr)

5 year Weight Loss and Crevice Sample CDFs TSPA Implementation of Crevice Data using unbounded Weibull distributions

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5 10 15 20

General Corro$ion Rate (nmyear)

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Corroborative corrosion rate data typically exhibit rates higher than the 5year data (at shorter exposure times)

Reference Corrosion Behavior Reported

Baker 1998 [DIRS 154510] Alloy 600 under atmospheric conditions 8 nmyr after 36 years of exposure

McCright 1998 [DIRS 114637] Alloy C-4 in marine atmospheric environment no visually apparent degradation after 50 years

Smailos 1993 [DIRS 168164] Alloy C-4 at 150C in NaCI-rich brine 70 nmyr at 12 months and 60 nmyr at 18 months

Exposure Time Mean Rate (Ilmyr) Sources(years) (days)

00027 1 0460 Lian el al 2002 [DIRS 164856] Table 3 potentiostatic polarization technique at 100 mV versus SSC applied potential in SAW 90DC N2 purQe

00027 1 1250 Lian et al 2002 [DIRS 164856] Table 3 potentiostatic polarization technique at 100 mV versus SSC applied potential in SCW 90degC N2 purge

0019 7 0100 Evans and Rebak 2002 [DIRS 164857] Figure 2 polarization resistance technique after one week in open-circuit potential in SAW 90 Q C air purge

0154 56 0182 Hua and Gordon 2004 [DIRS 171013J calculated from regression fit for 56-day weight-loss in SSW CR (MPY) = 313exp(-25300RT)

050 183 0076 LL990610605924079 [DIRS 104994J 599359_032 DATA REPORT (weightshyloss) and 599359 031 DATA REPORT (crevice)

100 365 0025 LL990610605924079 [DIRS 104994J 599359_005 DATA REPORT (crevice data) and 599359 006 DATA REPORT (weiQht-loss data)

200 730 0014 LL000112205924112 [DIRS 141284J S00041_005 DATA REPORT (Combined crevice and weight-loss data)

500 1825 0007 Section 6433 Table 6-6 (Crevice data only)

Validation DTN M00706WPOBVALROOO file Figure 7-1xs

Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28-Feb-2008 OCRWM L~ad Laboratory for Repostory Systms

13

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The Project weight loss data are of similar magnitude to recent control data and observed cycle-to-cycle weight change from the analysis of the 5 year data

Time (years) Corrosion Rate (lmyr) Equivalent Weight Loss (g)

(based on crevice sample geometry)

0154 0182 00015

05 0076 00020

1 0025 00013

2 0014 00016

5 0007 00018

Feb-08 scoping test on Alloy 22 control coupons

00012 g weight loss after 2-3 cleaning cycles

Cycle to cycle weight change for 5 year weight-loss coupons

Significant number of trials resulted in weight loss between 00005 g and 00015 g

Cycle to cycle weight change for 5 year crevice coupons


Sandia National Laboratories Analysis ofAlloy 22 Weight Loss due to General Corrosion 28middotFeb-2008 OCRWM Lead Laboratory for RpOlHory SystftlnS

14

1JieTJroject weighT10ss data are of shnnar m3gn1tudeHtoHHireceHniiMHWWWiWiWWWWfW

control data and observed cycle-to-cycle weight change from the analysis of the 5 year data

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----+- 0 CA267 (water + aceton e) ~ DCA268 (water + acetone)02 ______ 0 GA32 (acid clean) --- DGA33 (acid clean)

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Weight change (g) DWiWWtWiiiWWtWilWiWWtWlbull gt Jjpoundmiddotl1 bullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullbullmiddotmiddotmiddotmiddotwrlwr

Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28-Feb-2008 OCRWM Lead lahoratory for RlpOSlory Systems

- Weightloss Samples from AMR I I I IO0 i I I

15

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Proposed approach to clarifying the disposition of the 5year weight loss data

bull A subset of the previously analyzed 5 year samples could be cleaned using multiple cleaning cycles to determine if additional weight loss is observed compared to the existing data set

- It is proposed that samples from the sew and SOW aqueous environments be analyzed as the cleaning procedure for these exposure conditions has been characterized using control samples

- It is proposed that six weight loss samples and six crevice samples from each environment be analyzed initially 24 total samples represents approximately 2000 of the previously analyzed 5 year samples

Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28-Feb-2008 OCRWM Lead Laboratory for Roposllcry Systems

16

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Background Introduction

bull The corrosion rate used in the TSPA-LA is based on corrosion test data from 5 year test specimens and generated in -FY01

The 95 year test specimens are being readied to provide new data that would presumably validate the TSPA-LA corrosion rate

bull In a technical review of the 5 year data and a review of the methodology a vulnerability was uncovered

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Sandia National Laboratories Analysis of Alloy 22 Weight Loss due to General Corrosion 28middotFeb-2008 OCRWM Lead Lahoratory for Repostory Systl1tlS

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16







16

Documents

Analysis of Alloy 22 Weight Loss due to General Corrosion