ML13319A670

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CCNPP-CHLE-007, Rev. G, Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant.
ML13319A670
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Site: Calvert Cliffs  Constellation icon.png
Issue date: 10/18/2013
From: Kinsey S
Constellation Energy Nuclear Group
To:
Office of Nuclear Reactor Regulation
Morgan N
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CCNPP-CHLE-007, Reg g
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COATINGS BENCH-TOP AUTOCLAVE EXPERIMENT TEST PLAN for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007, Revision g October 18, 2013 Prepared by: Reviewed by: Approved by:

Stephen Kinsey Andy Henni, Craig Sellers John Swailes Blake Stair, Tim Sande Tom Konerth

Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013 REVISION HISTORY LOG Revision Description a Initial draft b Incorporate initial review comments c Incorporate 7/25 comments from CCNPP, B. Stair d Incorporate Comments from NRC Public Meeting and CCNPP e Test coating provided in sq. in per liter; moved target alkyds to Table 1 and deleted Table 5; resolved duplicate references f Added other debris to tests; revised test suite to have two tests with alkyd coatings and two without coatings g Addressed comments to Rev. f from Sellers, Stair, and UIUC i

Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013 Table of Contents 1.0 Introduction ................................................................................................................................................................ 1 2.0 Purpose ......................................................................................................................................................................... 1 3.0 Experimental Plan .................................................................................................................................................... 1 4.0 Experimental Parameters ...................................................................................................................................... 2 4.1 Debris Quantities .................................................................................................................................................. 2 4.2 Chemistry Conditions ......................................................................................................................................... 3 4.3 Buffer ......................................................................................................................................................................... 3 4.4 Temperature Conditions ................................................................................................................................... 4 4.5 Solution Sampling ................................................................................................................................................ 5 4.6 Agitation................................................................................................................................................................... 5 4.7 Autoclave Materials ............................................................................................................................................. 5 4.8 Autoclave Volume ................................................................................................................................................ 5 5.0 Test Matrix ................................................................................................................................................................... 5 6.0 Chemistry Analysis ................................................................................................................................................... 6 7.0 Experimental Methods ............................................................................................................................................ 6 7.1 Material Preparation........................................................................................................................................... 6 7.1.1 Coatings .......................................................................................................................................................... 6 7.1.2 Fibrous Debris ............................................................................................................................................. 7 7.1.3 Reactive Materials ...................................................................................................................................... 7 7.2 Visual Examination .............................................................................................................................................. 7 7.3 Vacuum Filtration ................................................................................................................................................ 7 8.0 Report ............................................................................................................................................................................ 8 8.1 Introduction ........................................................................................................................................................... 8 8.2 Experiment Description .................................................................................................................................... 8 8.2.1 Facility ............................................................................................................................................................. 8 8.2.2 Experiment Input Parameters............................................................................................................... 8 8.2.3 Material Preparation ................................................................................................................................. 8 8.2.4 Autoclave Setup and Control ................................................................................................................. 8 8.3 Experimental Results.......................................................................................................................................... 9 8.4 Summary of Results and Conclusions .......................................................................................................... 9 8.5 References ............................................................................................................................................................... 9 8.6 Appendixes ............................................................................................................................................................. 9 9.0 References .................................................................................................................................................................. 10 List of Tables Table 1: Debris Sample Quantities ................................................................................................................................... 3 Table 2: Chemistry Conditions ........................................................................................................................................... 3 Table 3: Solution Temperature Profile ........................................................................................................................... 4 Table 4: Test Matrix ................................................................................................................................................................ 5 List of Figures Figure 1: Solution & Sump Analysis Of Record Temperatures ............................................................................. 4 ii

Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013

1.0 INTRODUCTION

Calvert Cliffs Nuclear Power Plant (CCNPP) is implementing a refined chemical effects test program to aid in resolving GSI-191. This refined chemical effects test program includes a number of experiments and tests to investigate different aspects of chemical effects. Included in this program are integrated chemical effects head loss tests intended to simulate temperature, pressure, fluid, and debris conditions in containment after a loss of coolant accident (LOCA).

CCNPP has a variety of potentially reactive materials in containment that must be considered in the refined chemical effects test program. Some of these materials may influence the dissolution or corrosion of other materials such that including them in the integrated tests can be considered non-conservative. Some materials may be sufficiently immune to dissolution and corrosion so that they can be excluded from the integrated tests.

The objective of this bench-top autoclave test plan is to investigate the dissolution and elemental release rates of coatings materials postulated to be delivered into the containment sump coolant pool post-LOCA. The results of this test will help determine which, if any, coatings material combinations are most appropriate for inclusion in the integrated chemical effects head loss tests for CCNPP.

2.0 PURPOSE The purpose of this document is to describe a bench-top autoclave experimental plan for the CCNPP CHLE program. This plan presents the material combinations for the experiments, the thermal and chemistry conditions for each experiment, and the approach to analyzing the results.

3.0 EXPERIMENTAL PLAN The experimental plan consists of a series of dissolution experiments in which potentially reactive coatings materials are exposed to high temperature fluid simulating the post-LOCA fluid chemistry and temperature in containment for a 168 hour0.00194 days <br />0.0467 hours <br />2.777778e-4 weeks <br />6.3924e-5 months <br /> period. The identification and concentration of dissolution products and characterization of any precipitates will be compared to determine if significant dissolution and elemental release of potential precipitants occurs. Analysis of the results will provide recommendations on coatings materials to include in the integrated tests including the possibility of recommending no coatings be included.

The fluid chemistry will be similar to the initial post-LOCA pool chemistry expected at CCNPP. A scaled quantity of NaTB buffer will be dissolved in the test chamber fluid to simulate the buffer in the plant.

Materials used in the test will be representative of the coatings that are used in CCNPP's containment and that may be submerged in the containment pool or exposed to containment spray Page 1 of 10

Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013 and which may be expected to dissolve and contribute to chemical effects. The material quantities will be scaled to approximate the ratio of the test fluid volume to the volume of the pool fluid times the surface area of the postulated failed alkyd coatings in the pool fluid.

CCNPP has a postulated pool volume of 66,300 cubic feet or 495,950 gallons of fluid in the pool and 7,534 square feet of alkyd coatings in containment. Assuming 100% of the alkyd coating fails and is submerged in the pool would create twice this exposed surface (front and back of the coating) in the pool. Therefore, the alkyd coating on test coupons to be used in the autoclave shall be Materials other than alkyd coatings used in the test will be representative of the materials submerged in the containment pool or exposed to containment spray and expected to dissolve and contribute to chemical effects in the initial days of the LOCA. These include destroyed insulation, concrete, latent debris, and other miscellaneous materials in containment. The material quantities will be scaled to approximate the ratio of the test fluid volume to the volume of debris materials immersed in the pool fluid or the surface area of solid materials exposed to pool at CCNPP.

4.0 EXPERIMENTAL PARAMETERS 4.1 Debris Quantities The total alkyd coatings and representative coating surface area for each alkyd coating assumed as representative for CCNPP are presented in Table 1. Other materials to be used in the tests are also specified in the table.

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Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013 Table 1: Debris Sample Quantities Coatings Debris Test Quantity References in2 per liter of test fluid Total Unqualified Alkyd Coating 1.156 1 and 2 Alkyd Manufacturer Coating Glidden Professional Alkyd 0.578 NA KRYLON Industrial Enamel 100 Series 0.578 NA Reactive Materials Metallic Aluminum 0.03 10 Galvanized Steel 8.6 11 ASTM B-152 Copper 11.0 11 ASTM B-466 Cupro-Nickel 0.13 11 Concrete 0.45 11 Marinite Board 2.6 8 Lead 0.03 8 Zinc 22.8 1&2 Insulation Debris Test Quantity References gram/Liter (g/L)

Transco Thermal Wrap or NUKON (LDFG) Fiber 1.16 8&9 Mineral Wool Fiber 0.11 8&9 Lead Shield Jacket 0.027 8&9 4.2 Chemistry Conditions The initial water chemistry to be used in the tests described in this test plan is specified in Table 2.

Table 2: Chemistry Conditions Deionized Water with Reference Boron Concentration (H3BO3) 2714 ppm as boron1 6 Lithium Hydroxide 0.75 ppm as lithium 6 4.3 Buffer Include 3.57 grams per liter sodium tetraborate decahydrate (NaTB) buffer (Reference 6). The buffer shall be added after the other materials and not before the fluid temperature has reached 195°F during the initial solution heat-up.

1 The 2714 ppm boron concentration is prior to the introduction of the NaTB buffer.

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Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013 4.4 Temperature Conditions The experiments will use the temperature profile presented in Table 3 and Figure 1+/-5°F

[Reference 3].

Table 3: Solution Temperature Profile Time (sec) Temp (°F) Time (sec) Temp (°F) 0 280 28,800 224 400 280 43,200 195 800 279 64,800 191 1,000 279 86,400 187 3,600 274 115,200 181 7,200 266 144,000 176 14,400 252 172,800 170 604,800 170 290 270 250 Temperature (F) 230 210 190 170 150 0 8 16 24 32 40 48 Time (Hrs)

Test Temperature AOR Sump Temperature Figure 1: Solution & Sump Analysis Of Record Temperatures Page 4 of 10

Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013 4.5 Solution Sampling The fluid solution in the autoclave shall be sampled every 12 hours1.388889e-4 days <br />0.00333 hours <br />1.984127e-5 weeks <br />4.566e-6 months <br /> and at the conclusion of each experiment. The samples shall be stored in containers fabricated from non-reactive and corrosion resistant materials. Samples shall be adequate for post test chemical analysis (Total Organic Carbon, Gas Chromatography -Mass Spectrometry, Liquid Chromatography-Mass Spectrometry, or other) but limited in volume to avoid significantly affecting total volume of fluid remaining in the autoclave.

4.6 Agitation The autoclave shall be agitated continuously throughout the experiment to facilitate fluid flow across the test materials. The means of agitation shall not physically contact the debris or reactive materials inside the autoclave.

4.7 Autoclave Materials Wetted materials of the autoclave should be type 316 stainless steel or other very corrosion resistant material. No silicate glass products may be used.

4.8 Autoclave Volume The autoclave shall have a minimum volume of five (5) gallons.

5.0 TEST MATRIX The experiment will be performed in accordance with the test matrix presented in Table 4. Please note that reactive materials and insulation debris are included but only alkyd coatings are included (i.e., no epoxy or inorganic zinc coatings) and that the test shall be repeated. Four simultaneous tests are acceptable.

Table 4: Test Matrix As Specified in Table 1 Test No.

Alkyd Coating Reactive Materials Insulation Debris 1 none X X 2 none X X 3 X X X 4 X X X Page 5 of 10

Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013 6.0 CHEMISTRY ANALYSIS The concentrations of the following elemental species, compounds, or organic materials shall be reported for each of the chemistry samples. The required range of these measurements shall be from 50 ppb (0.05 mg/L) to 1000 ppm (1000 mg/L). That is, concentrations less than 50 ppb may not be detected and no concentration is expected to exceed 1000 ppm.

1. Aluminum
2. Magnesium
3. Silicon
4. Zinc
5. Copper
6. Lead
7. Titanium Dioxide
8. Calcium Carbonate
9. Total Organic Carbon 7.0 EXPERIMENTAL METHODS Professional laboratory and safety practices shall be followed. Specific laboratory procedures used to implement the experiment shall be made available to Calvert Cliffs for review and comment.

The following specific experimental processes shall also be followed.

7.1 Material Preparation 7.1.1 Coatings Coatings coupons shall be prepared in accordance with the coatings manufacturer's instructions and spray coated both sides to the mid-range of the manufacturer's recommended dry film thickness. The coupons shall be minimum 1 inch by 6 inch stainless steel strips at least 16 gauge with surface preparation that conforms to SSPC-SP6/NACE 3 specifications or specific manufacturer's requirements if available. Appropriate primer (i.e., etch primer) may be required to coat stainless steel coupons with alkyd top coat. It is expected and required that the primer not contribute to or prevent the failure of the alkyd top coat. Furthermore, its materials shall not misrepresent CCNPP plant conditions.

Post-application curing of the alkyd coupons is required. Manufacturer's recommendations for elevated temperature cure shall be followed if any are available. If none are available, allow coated coupons to air dry for 2 hours2.314815e-5 days <br />5.555556e-4 hours <br />3.306878e-6 weeks <br />7.61e-7 months <br /> or until dry-to-handle followed by convection (not radiant) oven curing at 175°F for 4 hours4.62963e-5 days <br />0.00111 hours <br />6.613757e-6 weeks <br />1.522e-6 months <br />. These general guidelines are an amalgamation of several manufacturer's recommendations for rapid drying of alkyd coatings.

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Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013 The samples shall be suspended in the autoclave and secured to remain submerged in the experimental fluid and protected from the agitation device but exposed to the flow of fluid produced by agitation.

Photographs of the coatings materials before preparation and after weighing or measuring shall be provided. Photographs documenting any post test degradation of the coatings debris shall be provided.

7.1.2 Fibrous Debris Fibrous debris shall be prepared in accordance with Reference 12, with the exception of steps 6.5, 6.6 and 6.7, dried, and weighed to the quantity specified. The fiber samples will be placed in stainless steel mesh containers and secured to remain submerged in the experimental fluid and protected from the agitation mechanism. Photographs of the fiber before preparation, after weighing, and contained in the mesh container shall be provided.

7.1.3 Reactive Materials Coupons of metal reactive materials shall be prepared from 20 gauge or thinner flat plates. The coupons shall be suspended in the autoclave fluid so that both faces are fully exposed to the fluid.

Concrete coupons may be fresh concrete but must be chemically equivalent to the concrete used in containment at Calvert Cliffs. Marinite coupons will be cut from a solid piece of Marinite board. The concrete and Marinite coupons shall not include particles which can pass through a 16 mesh sieve.

The concrete and Marinite coupons will be placed in stainless steel 18 mesh containers and secured to remain submerged in the experimental fluid and protected from the agitation mechanism.

Photographs of the reactive materials before and after preparation shall be provided.

7.2 Visual Examination A thorough visual examination of the autoclave and coatings shall be performed. Any indications of precipitation or dissolution shall be documented. Special attention shall be paid to floating fluids, especially 'oily' film.

7.3 Vacuum Filtration At the conclusion of the 168 hour0.00194 days <br />0.0467 hours <br />2.777778e-4 weeks <br />6.3924e-5 months <br /> test, a final agitation shall be performed and a sample shall be extracted from the remaining fluid. Vacuum filtration shall be performed on this sample specifically looking for suspended precipitates. Normal laboratory practices for vacuum filtration shall be followed. Chemical analysis of the materials captured on the filter shall be performed (i.e., SEM-EDS or other).

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Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013 8.0 REPORT A formal report shall be provided documenting the performance of the experiment and the results of the experiment. The following topics shall be included in the report.

8.1 Introduction A brief introduction to the report shall be presented 8.2 Experiment Description A detailed description of the experiment shall be presented including at least the following sections.

8.2.1 Facility A comprehensive description of the experimental facility shall be presented with photographs. This shall include:

1) Autoclave(s)
a. Volume capacity
b. Wetted materials
c. Heating method
d. Agitation method
2) Temperature controls
a. Heat up rate
b. Cool down rate
3) Instrumentation and analysis equipment
a. Temperature
b. pH
c. Chemical Analysis (e.g., Mass spectrometry, Total Organic Carbon) 8.2.2 Experiment Input Parameters A detailed description of the input parameters for each experiment shall be presented.

8.2.3 Material Preparation The methods and processes for preparing fluid solutions and coatings debris samples shall be described and the results presented with photographs.

8.2.4 Autoclave Setup and Control The procedures used to setup the autoclave, control temperature conditions, take and store samples, and perform the chemistry analyses shall be described in detail.

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Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013 8.3 Experimental Results The results of each test shall be presented in individual sections. These sections shall include at least the following information.

1) Experimental parameters used
2) Actual temperature profile achieved
3) Results of chemical analysis of samples
4) Deviations and Nonconformance Reports
5) Results of visual examination
6) Photographs of notable observations as appropriate 8.4 Summary of Results and Conclusions A summary of results comparing the individual tests if the experiment will be presented and any conclusion drawn presented.

8.5 References Unique references used in the preparation of the report shall be presented. This test plan shall be included as a reference.

8.6 Appendixes Appendixes shall be provided including as a minimum the following:

1) Test Logs
2) Calibration Certificates/Records
3) Standards Certificates
4) Photographs Page 9 of 10

Coatings Bench-Top Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant CCNPP-CHLE-007 Revision g, October 18, 2013

9.0 REFERENCES

1. Design Calculation CA06938, Rev. 0002, Prediction of LOCA Coating Debris Loads on the Containment Sump Strainer.
2. Design Calculation CA07464, Rev. 0000, Prediction of LOCA Coating Debris Loads on the Containment Sump Strainer.
3. Design Calculation CA06774, Rev. 0002, Containment Response to LOCA and MSLB for Calvert Cliffs Units 1 and 2.
4. Design Calculation CA08048, Rev. 0000, MPR Calculation No. 0090-0267-01, Probabilistic Distribution of Boric Acid Concentration in Containment Building Sump Pool.
5. Design Calculation CA06963, "Mass of Sodium Tetraborate Decahydrate Buffer Required for Post LOCA Containment Building Sump pH Control", Revision 1.
6. Design Calculation CA0TBD, Rev. 0000, MPR Calculation 0090-0267-02: Probabilistic Distribution of pH in Containment Building Sump Pool.
7. ML080380214 NRC Staff Review Guidance Regarding Generic Letter 2004-02 Closure in the Area of Plant-Specific Chemical Effect Evaluations, Enclosure 3.
8. Design Calculation CA08045, Rev. 0000, ENERCON Calculation No. CNSCC016-CALC-002, Calvert Cliffs Debris Generation Calculation.
9. Design Calculation CA07067, Rev. 0000, GSI-191 Debris Transport Calculation.
10. Design Calculation CA06940, Rev. 0001, Computation of Aluminum and Marinite Board Debris Load Inputs for Containment Sump Strainer.
11. Design Calculation CA08046, Rev. 0000, CCNPP GSI-191 Copper and Galvanized Steel Quantity Calculation.
12. ZOI Fibrous Debris Preparation: Processing, Storage and Handling, Revision 0, Nuclear Energy Institute, October, 2011.

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