chemical effects autoclave experiment test plan …chemical effects autoclave experiment test plan...

CHEMICAL EFFECTS AUTOCLAVE EXPERIMENT TEST PLAN for Calvert Cliffs Nuclear Power Plant

CCNPP-CHLE-005, Revision 2 May 20, 2013 Prepared by: Reviewed by: Approved by: Craig D. Sellers Andy Henni, Steve Kinsey John Swailes Helmut Kopke, Tim Sande Tom Konerth

Chemical Effects Autoclave Experiment Test Plan for Calvert Cliffs Nuclear Power Plant

CCNPP-CHLE-005 Revision 2, May 20, 2013

i

REVISION HISTORY Log

Revision Description

0 Issue for initial experiment

1 Reduce aluminum concentration to 2x best estimate and revise boron & lithium concentrations to actual maximum concentrations.

2 Increased boron concentration to account for BAST discharge, reduced Lithium Hydroxide concentration, revised temperature profile, and increased level of prescriptive detail.



ii

Contents

1.0 Introduction ................................................................................................................................................................ 1

2.0 Purpose ......................................................................................................................................................................... 1

3.0 Overall experimental Plan ..................................................................................................................................... 1

4.0 Experimental Parameters ...................................................................................................................................... 2

4.1 Debris Quantities .................................................................................................................................................. 2

4.2 Reactive Material .................................................................................................................................................. 2

4.3 Chemistry Conditions ......................................................................................................................................... 2

4.4 Buffer ......................................................................................................................................................................... 2

4.5 Temperature Conditions ................................................................................................................................... 2

4.6 Solution Sampling ................................................................................................................................................ 4

4.7 Agitation ................................................................................................................................................................... 4

4.8 Autoclave Materials ............................................................................................................................................. 4

5.0 Test Matrix ................................................................................................................................................................... 4

6.0 Chemistry Analysis ................................................................................................................................................... 5

7.0 Experimental Methods ............................................................................................................................................ 5

7.1 Debris Preparation .............................................................................................................................................. 5

8.0 Report ............................................................................................................................................................................ 6

8.1 Introduction ........................................................................................................................................................... 6

8.2 Experiment Description .................................................................................................................................... 6

8.3 Experimental Results .......................................................................................................................................... 7

8.4 Summary of Results and Conclusions .......................................................................................................... 7

8.5 References ............................................................................................................................................................... 7

8.6 Appendixes ............................................................................................................................................................. 7

Attachment 1: NEI Fiber Debris Preparation Protocol ............................................................ 10 Pages

List of Tables

Table 1: Insulation Sample Quantities ............................................................................................................................ 2

Table 2: Reactive Material Quantities ............................................................................................................................. 2

Table 3: Chemistry Conditions ........................................................................................................................................... 2

Table 4: Solution Temperature Profile ........................................................................................................................... 3

Table 5: Test Matrix ................................................................................................................................................................ 4

List of Figures

Figure 1: Solution & Sump AOR Temperatures ........................................................................................................... 3



Page 1 of 8

1.0 INTRODUCTION

Calvert Cliffs Nuclear Power Plant (CCNPP) is implementing a risk-informed approach to resolving

GSI-191 that includes the performance of a number of chemical effects experiments. These

experiments are intended to simulate temperature, pressure, fluid, and debris conditions in

containment after a loss of coolant accident (LOCA).

Temperature conditions inside containment during the initial portion of a large break LOCA peak at

approximately 280°F. Simulating these temperature conditions in a chemical effects test requires

the use of a pressurized test facility. Elemental release estimates using the WCAP-16530

methodology indicate at a constant temperature of 195°F for 21 hours, the release of aluminum was

the same as the initial 10 hours at the analysis of record sump temperature. The same estimate

indicated a 69% increase in calcium release and a 25% increase in silicon release.

The objective of this autoclave test is to validate the WCAP-16530 release estimate and to

investigate whether maintaining the test temperature at 195°F for an extended time adequately

simulates the elemental release from prototypical materials during the initial 10 hours of a design

basis LOCA at CCNPP. The results of this test will influence the decision on how to simulate the high

temperature portion of the accident profiles in the CCNPP Chemical Effects Head Loss Experiment

(CHLE) program.

2.0 PURPOSE

The purpose of this document is to describe the autoclave experiment planned for the CCNPP CHLE

program. This plan presents the sequence for performing the experiment and the conditions for

each experiment.

3.0 OVERALL EXPERIMENTAL PLAN

The overall concept for the experiment is eight corrosion experiments, four using a temperature

profile similar to the initial 10 hours of the design basis LOCA at CCNPP and four maintained at

195°F for 24 hours, with fluid simulating the post-LOCA fluid solution in containment and

corrodible materials expected in containment in the fluid. The identification and concentration of

corrosion products and characterization of any precipitates will be compared to determine if there

is a significant difference in corrosion and elemental release at two temperature conditions.

Materials 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 10 hours of the LOCA. These include destroyed insulation, concrete, latent debris and

other miscellaneous materials in containment. The material quantities will be scaled to



Page 2 of 8

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.

The fluid chemistry will be similar to the initial post-LOCA pool chemistry expected at CCNPP. A

scaled quantity of NaTB buffer will be allowed to dissolve in the test chamber to simulate the

dissolution of buffer in the plant.

4.0 EXPERIMENTAL PARAMETERS

4.1 Debris Quantities

Table 1: Insulation Sample Quantities

Insulations Debris Test Quantity Reference Transco Thermal Wrap or NUKON (LDFG) Fiber 1.10 gram/Liter (g/L) 1 & 2 Mineral Wool Fiber 0.30 g/L 1 & 2

4.2 Reactive Material

Table 2: Reactive Material Quantities

Material Description Test Quantity Reference

Metallic Aluminum 0.03 in2/L 3 Galvanized Steel 7.5 in2/L 4 Copper 11.8 in2/L 4 Exposed Concrete 0.1 in2/L 4 Marinite Board 2.75 in2/L 1

4.3 Chemistry Conditions

Table 3: Chemistry Conditions

Deionized Water with Reference Boron Concentration (H3BO3) 2800 ppm as boron1 6 Lithium Hydroxide 0.78 ppm as lithium 6 Initial pH ~5 N/A

4.4 Buffer

Include 3.78 grams per liter sodium tetraborate decahydrate (NaTB) buffer. 4.5 Temperature Conditions

Four experiments will be maintained at 195°F ±5°F for 24 hours.

1 The 2800 ppm boron concentration is prior to the introduction of the NaTB buffer.



Page 3 of 8

The other four will simulate the temperature profile presented in Table 4 and Figure 1 ±5°F [Ref. 5].

Table 4: Solution Temperature Profile

Time (m) Temp (F)

0 280.0

10 280.0

60 271.5

120 263.0

180 254.5

240 246.0

300 237.5

360 229.0

420 220.5

480 212.0

540 203.5

600 195.0

Figure 1: Solution & Sump AOR Temperatures

190.0

200.0

210.0

220.0

230.0

240.0

250.0

260.0

270.0

280.0

290.0

0 100 200 300 400 500 600

Tem

pe

ratu

re (

F)

Time (Minutes)

Autoclave Temp (F) AOR Sump Temp(F)



Page 4 of 8

4.6 Solution Sampling

The fluid solution in the autoclave shall be sampled periodically as specified in the Test Matrix and

at the conclusion of each experiment. The samples shall be stored in containers fabricated from

non-reactive and corrosion resistant materials.

4.7 Agitation

The autoclave shall be agitated continuously throughout the experiment to facilitate fluid flow

across the contained materials.

4.8 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.

5.0 TEST MATRIX

The experiment will be performed in accordance with the test matrix presented in Table 5.

Table 5: Test Matrix

Test No. Materials/Chemicals Included

Temp (F) Duration Sample Times Table 1 Table 2 Table 3

1 No No Yes Table 4 10 hours 10 hours

2 No No Yes 195 ±5 24 hours 24 hours

3 Yes Yes Yes Table 4 10 hours 10 hours



6 Yes Yes Yes 195 ±5 24 hours 16, 18, 20,

22, & 24

hours

7 Yes Yes Yes 195 ±5 24 hours

8 Yes Yes Yes 195 ±5 24 hours



Page 5 of 8

6.0 CHEMISTRY ANALYSIS

Mass spectrometry of the fluid used in the experiment shall be performed:

1. On the deionized water prior to addition of the boric acid at the beginning of each

experiment, and

2. On the fluid solution collected during each experiment.

The concentrations of the following elemental species shall be reported:

1. Aluminum

2. Boron

3. Calcium

4. Chromium

5. Iron

6. Magnesium

7. Nickel

8. Molybdenum

9. Phosphorus

10. Silicon

11. Sodium

12. Sulfur

13. Zinc

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 Debris Preparation

7.1.1 Fibrous Debris

Fibrous debris shall be prepared in accordance with Attachment 1 [Ref. 7], with the exception of

steps 6.6 and 6.7, dried, and weighed to the quantity specified. The water used for soaking in step

6.5 of Attachment 1 shall be deionized water. 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.



Page 6 of 8

7.1.2 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 or chipped from masonry block. 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.

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. Mass Spectrometry



Page 7 of 8

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 corrosion 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.

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) 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



Page 8 of 8

9.0 REFERENCES

1. Design Calculation CA0xxx, Rev. 000y, ENERCON Calculation No. CNSCC016-CALC-002, Calvert

Cliffs Debris Generation Calculation.


Cliffs Risk-Informed Debris Transport Calculation.

3. Design Calculation CA06940, Rev. 0001, Computation of Aluminum and Marinite Board Debris

Load Inputs for Containment Sump Strainer.


Cliffs Containment Metal Calculation.

5. Design Calculation CA06774, Rev. 0002, Containment Response to LOCA and MSLB for Calvert

Cliffs Units 1 and 2.

6. Design Calculation CA0xxx, Rev. 000y, MPR Calculation No. 0090-0269-01, Post-LOCA

Containment Pool Boron, Lithium Hydroxide, and Silica Concentrations.

7. “ZOI Fibrous Debris Preparation: Processing, Storage and Handling,” Revision 0, Nuclear

Energy Institute, October, 2011.



Page 1-1 of 1-10

Attachment 1

NEI Fiber Debris Preparation Protocol

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