ELECTROCHEMICAL STUDY OF CORROSION PHENOMENA IN ZIRCONIUM ALLOYS
by
Nicole M. Treeman
Lieutenant, United States Navy
B.S. Civil Engineering 1997
Worcester Polytechnic Institute
Submitted to the Department of Nuclear Engineering
in Partial Fulfillment of the Requirements for the Degrees of
Nuclear Engineer's Degree
and
Master of Science in Nuclear Engineering
at the
Massachusetts Institute of Technology
June 2005
© Massachusetts Institute of Techl)ology,2005. All rights reserved.
ARCHIVES
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Signature of A LUIUor;
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Certified by:
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Department of Nuclear Engineering
May 20, 2005
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Ronald G. Ballinger, Sc.D.
Professor of Nuclear Science and Engineering and Material Science and Engineering
Thesis Supervisor
Certified by:
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Ronald M. Latanision, Ph.D.
Professor Emeritus of Material Science and Engineering
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ThesisReader
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Accepted by:
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Jeffrey A. Coderre, Ph.D.
Associate Professor of Nuclear Science and Engineering
Chairman, Committee for Graduate Students
ELECTROCHEMICALSTUDY OF CORROSION PHENOMENAIN ZIRCONIUM ALLOYS
by
Nicole M. Treeman
Submitted to the Department of Nuclear Engineering
on May 20, 2005 in Partial Fulfillment of the
Requirements for the Degrees of
Nuclear Engineer
and
Master of Science in Nuclear Engineering
Abstract
Shadow corrosion of zirconium alloy fuel cladding in BWR environments, the
phenomenon in which accelerated corrosion is experienced when the cladding surface is in close
proximity to other metals, has become a potentially life-limiting issue for BWR fuel. Recent
results from experimentation at MIT, Halden, and Studvik suggest that a galvanic coupling
drives the phenomenon between the cladding and the adjacent material. However, the actual
processes involved are not understood. One key parameter that would help in the understanding
of the phenomenon would be a measurement of the actual corrosion current between fuel
cladding and adjacent materials in the actual in-reactor environment.
The limitations placed on the bum-up of uranium oxide fuel correlates to the amount of
corrosion seen through a directly measurable oxide thickness on the waterside of the zirconium
alloy cladding. This oxide corrosion product directly correlates to distance from structural
components, leading to the effect commonly referred to as shadow corrosion. In recent
experiments, Studvik determined that there are large ECP differences associated with Inconel
and zirconium alloys that correlate to increased galvanic current density when the materials are
coupled.
In this thesis research, four electrode pairs were used to measure galvanic current
densities in the irradiation environment: Pt-Pt, Zircaloy 2 (Zr-2)-Pt, Inconel (X-750)-Pt, and Zr2-X-750. To determine the changes in the coolant water conductivity due to the presence of
radiolysis products, electrochemical potential measurements of Pt-Pt coupled electrodes were
analyzed. Finally, attempts to characterize the observed oxide behavior using measurements
from Electrochemical Impedance Spectroscopy (EIS), also known as Alternating Current
Impedance, were conducted.
Through the measurements taken, analysis of the mechanisms potentially causing the
shadow corrosion phenomenon was conducted. The results of the observations included:
· Measurement of increased conductivity of coolant water correlating to increases in
reactor power.
· Measurement of increased galvanic current measurements correlating to increases in
reactor power.
Thesis Supervisor: Ronald G. Ballinger
Title: Professor of Nuclear Engineering and Material Science and Engineering
3
Dedication and Acknowledgements
This experiment would not have been possible without the initial hypothesis and
experimental design of II Soon Hwang of Seoul National University. His guidance and patience
in mentoring my early understanding of electrochemical affects of corrosion and alternating
current impedance were instrumental in the execution and analysis of this experiment.
The funding for this experiment was provided by Electric Power Research Institute, Inc.
(EPRI) and Kurt Edsinger.
I also extend my gratitude to Kevin Miu for his assistance with the initial Visual Basic
programming and Pete Stahle for his revisions to the program during in-core experimentation. I
would also like to thank Pete for his assistance in design, assembly, and installation of the
experimental assembly. Additionally, the in-core experimental support, along with advice
regarding handling radiological material, of Dr. Gordon Kohse and Yakov Ostrovsky greatly
broadened my scope of knowledge.
I would also like to thank the Nuclear Reactor Operations staff, particularly Ed Lau, for
their support during experimentation. I would also like to thank the Reactor Radiation Protection
Program staff, Fred McWilliams, Beth Rice, Doug LaMay, and Rich Dresios, for their assistance
in training me for reactor access to conduct experimentation, radiation safety, and activity
calculations for the experiment approval.
Finally, I would like to express my deepest gratitude to Professor Ron Ballinger. His
direct and candid guidance greatly shaped this experiment and my MIT experience. His ability
to instill confidence enabled me to obtain my educational goals at MIT. I look forward to his
interaction with my future career in Navy Nuclear Power.
I dedicate this manuscript to my husband, Loren Reinke, and our daughter, Ariadne
Treeman-Reinke. Your unending support, understanding, and love gave me the strength and
courage to obtain my goals. I am truly blessed and thankful to have you in my life.
4
Table of Contents
ABSTRACT
..................................................................................................................................................
DEDICATION AND ACKNOWLEDGEMENTS ....................................
.............................
3
4
TABLE OF CONTENTS ........................................................................................................................... 5
1.
INTRODUCTION
1.1.
1.2.
1.3.
1.3.1.
1.3.2.
1.3.3.
1.3.4.
1.4.
AND BACKGROUND .......................................
................ .......................
ZIRCONIUM IN THE NUCLEAR INDUSTRY ........................................
.........................
DEFINITION OF THE SHADOW CORROSION PHENOMENA ..............................................................
METALLURGICAL BACKGROUND ...................................................................................................
STRUCTURAL AND COMPOSITIONAL PROPERTIES OF ZIRCONIUM ALLOYS ..................................
HISTORY OF USE OF ZIRCONIUM ALLOYS AS NUCLEAR FUEL CLADDING. ...............................
IDENTIFIED LIMITATIONS OF ZIRCONIUM ALLOYS IN NUCLEAR ENVIRONMENTS ........................
CURRENT TRENDS OF IMPROVEMENT IN ZIRCONIUM ALLOYS .....................................................
IMPACT ON DESIGN AND LICENSING ..............................................................................................
]1.5. NRC CONCERNS.........................................
8
8
9
10
10
12
13
15
16
]1.7. NRC DOCUMENTATION.........................................
17
18
19
][.8.
11.9.
21
21
][1.6. PAST DEVELOPMENTS IN UNDERSTANDING THE SHADOW CORROSION PHENOMENA ............
THESIS PROBLEM DESCRIPTION .........................................
OUTLINE OF THIS THESIS ................................................................................................................
1.10.
2.
REFERENCES..................................................................................................................................
ELECTROCHEMICAL
ANALYSIS .................................
.......
22
25
2.1.
2.2.
2.3.
ELECTROCHEMICAL POTENTIAL ...................................................................................................
GALVANIC CURRENT ......................................................................................................................
ALTERNATING CURRENT IMPEDANCE .................................
25
26
27
2.4.
REFERENCES
.................................
31
3.
3.1.
EXPERIMENTAL DESIGN ............................................................................................................ 32
DESIGN OF THE ELECTROCHEMICAL MEASUREMENT ASSEMBLY AND EXPERIMENT .............. 33
36
3.1.1. ELECTROCHEMICAL MEASUREMENT EQUIPMENT .........................................................................
3.2. COMPUTERPROGRAMS.........................................
38
3.3.
EXPERIMENTATION IN LABORATORY ENVIRONMENT .................................................................
39
3.4.
3.5.
MITR-2 CHARACTERISTICS
...........................................................................................................
REFERENCES............................ ........................................................................................................
40
45
4.
5
EXPERIMENTAL RESULTS AND DISCUSSION ...........................................
46
4.1.
4.2.
4.3.
4.4.
4.5.
5.
5.1.
5.2.
GALVANICCURRENT DATA GATHERED..........................................
CONDUCTIVITYDATA GATHERED..........................................
46
48
GALVANIC CURRENT AND CONDUCTIVITY ANALYSIS ..........................................
OBSTACLES ENCOUNTER DURING EXPERIMENTATION ..........................................
52
53
REFERENCES.
.........................................
56
CONCLUSIONS ..........................................
57
REITERATION OF HYPOTHESIS .........................................
57
COMPARISON OF EXPERIMENTAL RESULTS WITH EXPECTED RESULTS .................................... 57
APPENDIX A - PT-PT COIIPLE,EGRAPHS
V V YU
1 _ 1 1~~~~1__
_ _ _ _ _ _ _ _ _~~~1
1 111111 11~--
----- -- --------------
.59
APPENDIX B - ZR-PT COUPLE GRAPHS ......................................................................................... 77
APPENDIX C - X750-ZR COUPLE GRAPHS ...................................
APPENDIX D - X750-PT COUPLE GRAPHS ...................................
.....
95
113
APPENDIX E - ECP DATA .................................................................................................................. 131
APPENDIX F - GALVANIC DATA .................................................................................................... 134
6
'Listof Figures
Figure
Figure
Figure
Figure
Figure
Figure
Figure
Figure
Figure
Figure
Figure
Figure
Figure
1.1 Zr-O Phase Diagram [1.6] .......................................................................
11
2.1 Ideal Nyquist Plot ........................................................................
29
2.2 Ideal Bode Plots ........................................................................
30
3.1: Top down view of specimen arrangement in module [3.1] .................................................................33
3.2: Side view of specimen arrangement in module [3.1]........................................................................ 35
3.3: Electrochemical monitoring equipment arrangement ....................................................................... 37
3.4 Reactor Top [3.2 ..................................................................................................................................... 40
3.5 Coolant Flow through Rig (Note: Not to scale) ........................................................................
42
3.6 Letdown system from experimental assembly to recirculation pump [3.1]........................................43
3.7 Charging tank, letdown monitoring equipment, and chemistry control area ....................................44
4.1 Galvanic Current V. Reactor Power ........................................................................
46
4.2 Zircaloy-2 Resistance V. Time in Reactor ........................................................................
47
4.3 Resistivity Comparison between Zircaloy- 2 and X-750 at 4 MW ......................................................48
Figure 4.4 Pt-Pt correlation chart ........................................................................
Figure
Figure
Figure
Figure
Figure
4.5
4.6
4.7
4.8
4.9
49
Coolant Conductivity, as measured by Pt-Pt electrode, V. Reactor Power ........................................50
Letdown Conductivity Measurement V. Reactor Power .....................................................................51
Coolant Conductivity, as measured by Pt-Pt electrode, V. Time at 4 MW Power ............................52
Zr-2-Pt M easured Galvanic Current V. Pt-Pt Measured Conductivity .............................................53
Zr-2-X-750 Measured Galvanic Current V. Pt-Pt Measured Conductivity ....................................... 53
List of Tables
Table 1.1 Alloying elements in Zircaloy 2 and 4 ......................................................................
Table 1.2: Thermal properties of Zircaloy 2 (a phase) [1.13] ........................................................................
Table 4.1: Experimental Conditions ........................................................................
7
11
17
55
1. Introduction and Background
1.1.
Zirconium in the Nuclear Industry
As the nuclear industry grew into a feasible and economical means of providing power
for the propulsion of Navy ships and submarines, electrical generation for municipal and
industrial use, and innovative means for medical and scientific research, requirements for
improving the fuel used arose. Due to natural availability, uranium was the chosen fuel;
however, it suffered from significant limitations. Uranium in pure form, like many metals, is
highly reactive, particularly in the aqueous environment expected in a nuclear reactor [ 1.1]. The
high rate of corrosion experienced by uranium, possibly leading to flaking of oxidized particles
that potentially can become entrained in the water cycle of a nuclear reactor leading to
widespread contamination issues, lead to the exploration of uranium dioxide (UO2) as fuel.
While U0 2 is far less reactive, since oxidation has already taken place, a new concern arose.
This concern relates directly to the fission process and containment of radioactive fission
products.
During the fission process, the binding energy of an atom changes due to the energy of
the interacting neutron. Neutron interaction can lead to the original (parent) atom either splitting
into two new atoms, with the release of a subsequent neutron to decrease the Z - number (the
sum of the neutrons and protons in the atomic nucleus) back to more stable value, or in the form
of decay. There are three primary forms of decay: a,
energy photons.
a,
and y. y- decay is the emission of high-
- decay is the emission of an electron or positron for which the Z- number of
the atom remains constant, but the atomic (A) number increases or decreases by one. The
predominant decay is -P - decay, or electron emission. The final decay type is a - particle
emission, in which a 4 He ion is released. In each of the decay processes, the created (daughter)
atom may be unstable, leading to subsequent decay of various elemental isotopes with
independent properties.
Due to the various properties of the parent and daughter atomic isotopes, it became
important to be able to isolate the fission products from the remainder of the plant systems and
external environment. The proposed means was to sheath the fuel in a second, non-reactive alloy
with high corrosion resistance and low neutron affinity. The two alloys recommended were
stainless steel and zirconium. Both alloys provided high corrosion resistance and the ability to
withstand the high temperatures and stresses present within a nuclear reactor. However, stainless
steel has a significantly higher affinity for thermal neutrons, meaning that more uranium would
need to be fissioned to create enough neutrons to sustain required reaction rates [1.1]. Based
predominantly on this fact, zirconium alloys were chosen to sheath, or clad, the fuel.
With the increasing demand for cleaner, efficient, and more reliable forms of energy, the
nuclear industry continues to explore ways to maximize the utilization of fuel while minimizing
the amount of hazardous waste produced. With innovative fuel management schemes
developing to match current burn-up allowances, the nuclear industry continues to seek safe
means to increase burn-up. One of the limiting factors for fuel burn-up is the amount of
corrosion of the zirconium alloy cladding. This corrosion occurs in several forms, but one
unique form of particular interest is the so-called shadow corrosion.
1.2. Definition of the Shadow CorrosionPhenomena
One of the potentially most system limiting forms of zirconium alloy corrosion is shadow
corrosion. Shadow corrosion is a localized form of "normal" oxidation in which the rate of
oxidation is accelerated due to the presence of a "shadowing" material in proximity in an
irradiation environment. However, the causes of shadow corrosion continue to elude scientists
9
and industry managers alike, first identified over three decades ago. Observations of metallic
materials near the Zircaloy indicate that the Zircaloy is often less noble than the corresponding
metallic structure and the corresponding corrosion mirrors the form of the more noble
component [1.2].
In early investigations of shadow corrosion, the phenomena appeared to be closely
related to common nodular corrosion. Nodular corrosion, in BWRs, is attributed to the radiolysis
and boiling process enabling oxygen accumulation in the environment. However, nodular
corrosion is greatly reduced with rigorous control of second-phase particle size and adjustment
of annealing times after a late O-quenchduring cladding fabrication [1.3].
1.3.
Metallurgical Background
1.3.1. Structural and Compositional Properties of Zirconium Alloys
Zirconium use as cladding material in nuclear reactors emerged in the mid-1950s and
expanded rapidly as commercial water reactors entered the power industry [1.4]. Pure zirconium
exhibits characteristics that make it a desirable choice for use as a material in nuclear reactors.
However, zirconium has high reactivity with oxygen and, in the form used for fuel cladding,
exhibits a strongly anisotropic hexagonal close packed (HCP) crystal structure. Pure zirconium
at room temperature and pressure crystallizes an a phase of the hexagonal close packed structure
[1.5]. Figure 1.1 shows a Zr-O phase diagram. The phase diagram indicates that at the expected
operational temperatures of 288°C, zirconium remains in the a phase. The lattice parameters for
the a phase are a = 3.2312 A and c = 5.1477 A. The P phase of zirconium is body centered
cubic, and begins to form at the grain boundaries of the a phase crystals when the metal is heated
above 866°C [1.7]. The lattice parameter for the P phase of zirconium is a = 3.6090 A [1.8].
10
Figure 1.1 Zr-O Phase Diagram [1.6]
Atomllic F'rrce-l:
P:. 1
_
aL .
I;>-J I -
,
(oZr)
'
.r
i
'
.
~ e/ t
---IjZr
i$ ~q'YF,~
*"i'd,,"
,-------
-ads
'Zf~
.
!
.I~~~
Table 1.1 [1.8].
xviyclnE
,
VWih
Inrc s.
---..--
,,,,, _____sI/.l~,lh
| _']en
I
'i
._..
l
)X.'tll
However, pure zirconiumChromium
is soft and demonstrates lower corrosion resistance than
stainless steel alloys in high temperature, aqueous environments due to the oxide becoming nonadherent. In order to improve the expected
alancloyse
performance of zirconium,
Balancreated
to
improve yield and tensile strength, as well as corrosion resistance [1.9]. The most commonly
used zirconium alloys are Zircaloy 2 or 4, for which the chemical compositions are provided in
lable 1.1 [1.8].
Table 1.1 Alloying
elements in Zircaloy 2 and 4
Alloying Element
Zircaloy 2 (weight %)
Zircaloy 4 (weight %)
Tin
1.20 - 1.70
1.20 - 1.70
hon
0.07 - 0.20
0.18 - 0.24
Chromium
0.05 - 0.15
0.07 - 0.13
Nickel
0.03 - 0.08
Zirconium
Balance
11
.
...
Balance
Both Zircaloy 2 and 4 exhibit recrystallized microstructures at room temperature that
consist of equiaxed grains (equal size in all three orthogonal directions) of a phase Zr with Sn in
solid solution and the other alloying elements forming intermetallic compounds with Zr [1.8].
The deficient properties experienced in using pure zirconium as cladding are remedied through
using the alloying elements. Some elements earlier thought to be impurities also impact some of
the deficiencies of using pure zirconium. The addition of tin to the Zircaloy aids in the a phase
stabilization, increases corrosion resistance, and strengthens the alloy. The remaining alloying
elements, iron, chromium, and nickel, also promote corrosion resistance. Several elements
originally thought to act solely as impurities in Zircaloy are oxygen, carbon, and silicon. Oxygen
has since been found to serve as a solid solution strengthener and a phase stabilizer. During 13
heat treatments, carbon helps in attaining the right texture, while silicon results in improved
corrosion resistance [1.8]. Given the expected nuclear reactor environment of 250-350°C, with
pressures nominally around 7 MPa for boiling water reactors (BWRs) and 15 MPa in pressurized
water reactors (PWRs), it can be expected that zirconium alloys will remain in the a phase, or
hexagonal close packed structure.
1.3.2.
History of Use of Zirconium Alloys as Nuclear Fuel Cladding
As nuclear power gained momentum, designs emerged utilizing water as a coolant and
moderator. Despite the lower reactivity of UO2 as a fuel, concerns remained about containment
of the fission and corrosion products in the coolant. Initial decisions regarding the use of a
second material to serve as a protective sheath evolved. The characteristics of the sheathing
material stemmed from required performance criteria: good operational performance in a high
temperature, aqueous environment; low susceptibility to corrosion in a high temperature,
12
aqueous environment; and low absorption cross section for thermal-spectrum neutrons.
Zirconium was one of the of elemental metals meeting these requirements [1.9].
Initial tests indicated that zirconium corrosion behavior depended on the orientation of
the individual grains or texture of the material. The fabrication texture resulted in regions of
nodular corrosion predominantly on grain boundaries between two grains demonstrating lower
oxidation rates. Ulsingtransition metals to alloy the zirconium reduced the occurrence of nodular
corrosion, leading to the development of a more uniform oxide layer less susceptible to spalling
[1.3].
With the trends to reactor designs requiring higher temperatures and pressures, and the
economics of operating reactors driving operators to push for higher burnups and hence
enrichments, the NRC continues to investigate the limitations of current claddings. While Zrbiased alloys do have significant neutronic advantages compared to stainless steels, the more
extreme operating conditions, coupled with the limitations from shadow corrosion and other
means of corrosion, cause concern from a regulatory standpoint. Changes in the properties of the
cladding include embrittlement, higher internal pin pressure from built up fission product gases,
and fuel expulsion during reactivity initiated accidents. The nature of these limitations derives,
in significant part, from the limitations of the zirconium alloys.
1.3.3. Identified Limitations of Zirconium Alloys in Nuclear Environments
One of the elements originally considered an impurity was oxygen. This element greatly
affects the slip behavior of the alloy in proportion to its concentration within the matrix.
However, the interaction of the aqueous environment is important to create the oxide layer that
serves as protection from further corrosion. This oxide layer creates a passive region resistant to
corrosion, but reduces the amount of base material in the cladding. This reduction in the original
13
alloy thickness is further aggravated by cracking of the protective oxide layer, leading to
increased localized corrosion. The creation of this oxide layer also creates vacancies within the
base alloy, potentially leading to changes in the mechanical properties of the alloy. The
concentration of vacancies leads to increased diffusion paths for strained atoms leading to higher
creep rates. This creep can lead to excessive plastic deformation.
The injected vacancies from the removal of a metal ion into the oxide layer have multiple
potential paths. One is in-situ vacancy annihilation at the oxide/alloy interface. If this
annihilation does not occur, then the vacancy may precipitate out and can contribute to void
formation [1.10]. The voids created, or grown, affect the corrosion resistance, mechanical, and
thermodynamic properties of the alloy. This includes elevated levels of oxygen in the alloy just
beneath the oxide layer leading to reduced ductility and fracture toughness [ 1.11].
In addition to the elevated levels of oxygen, irradiation of zirconium alloys creates
"black-dot," or clusters of irradiation created, defects, small dislocation loops, short line
dislocations, and dislocation entanglements [1.11]. The three dislocation related defects occur
on the prismatic plane with an <a> - type Burgers vector at lower fluences, and associated fuel
burnup. Burnup is the measurement of the amount of fissile uranium consumed during the
fission process. At higher burnups (fluence), there is an increase in mechanical disturbance
leading to breakaway oxidation, breakaway creep and growth, decreases in ductility, and
increases in brittle-type fracture behavior [1.11].
The exposure of metallic materials in the nuclear environment can lead to unique
phenomena. A crystal lattice can be easily described as atomic nuclei occupying lattice sites
with a sea of electrons filling the remaining volume. This configuration allows for entrance of
alpha particles and high-energy neutrons into the lattice. The alpha particles tend to congregate
14
in regions around voids and other defects leading to pockets of helium and alteration of creep
behavior within the crystal.
The high-energy neutrons, in the simplest sense, act like a billiard ball striking one
nucleus and potentially jarring it loose from its lattice site. This now-free atom may interact with
other lattice sites or become a self-interstitial.
In either case, this potentially raises the energy of
the crystal and leads to easier corrosion of the lattice.
As an alloy is exposed to a flux of high-energy particles, displacement of the original
elements creates dislocations and other crystalline defects affecting the mechanical and
crystalline properties of the alloy. With oxidation creating the potential for supersaturation of
vacancies in the base alloy, along with collection of vacancies into voids, and increasing the
oxygen content in the region below the oxide layer, the properties of the alloy greatly change
with increased fuel burnup. The natural corrosion, exacerbated by the impinging high-energy
neutrons, also enables diffusion of hydrogen into the alloy creating embrittlement or diffusion of
fission products into the overall system or environment. While the processing of the alloy
cladding is accomplished to align the texture for best strength and desired properties, including
annealing to reduce initial existing defects, there are other means of improving the alloy itself.
Through exploration of different alloying compositions with elements added to assist in
corrosion resistance and diffusion mitigation, the goal of developing a clad material allowing for
higher burnup and higher fuel efficiency may be achieved.
1.3.4. Current Trends of Improvement in Zirconium Alloys
While general corrosion is alleviated through the tailoring of precipitates and other
characteristics of the alloy, there have been observances of increased localized corrosion. This
corrosion has been partially reduced through additions of various alloying elements that change
15
the precipitates formed. One of the emerging elements is Nb, which reduces localized corrosion
through preferential corrosion of precipitates, dependent on the amount of Nb added with respect
to the saturation levels within the alloy [1.12].
Many of the traditional means of altering the crystalline structure through annealing, cold
working, and/or quenching fail to maintain long-term viability in the nuclear environment. The
fluctuations of thermal stresses from different operational states create dynamic situations with
regard to failure mechanisms, such as creep, and creation of means for greater dislocation
interaction potentially changing the material through hardening mechanisms, creation of FrankReed sources, or diffusional paths for impurity atoms. The interaction with impinging neutrons
and alpha particles leads to the creation of vacancies and interstitials, along with their affects on
structure and mechanical properties. These neutrons may also interact with water creating
radiolysis products, potentially changing the water chemistry in LWR coolant channels.
1.4. Impact on Design and Licensing
The fuel costs per fuel cycle derive from the cost of yellowcake and processing. Once
the facility is built and operating within design capacity, the cost of processing remains constant,
the changes in fuel costs remain primarily dependent on the price for yellowcake the
manufacturer paid. Typical fuel cycles center on a refueling period ranging from 12 to 24
months, with the majority operating with an 18-month period. Dependent on the minimization of
the number of required shutdowns for refueling, and maximization of fuel bum-up, the
percentage of the fuel rods replaced also varies.
Typical water-cooled reactor designs include fuel enrichment around 3% U-235, with the
balance principally comprised ofU-238 [1.13]. American enrichment plants typically use a
gaseous diffusion process. After the fuel is entered into the reactor core for two to three
16
refueling cycles, depending on the planned rotation, the bum-up limit prior to discharge is driven
by the average bum-up of the peak rod, set at 60 gigawatt-days per ton of heavy metal [1.14].
In addition, the NRC imposes limitations over the operation of the reactor. These
]limitations,imposed to assure safety of the overall system including cladding, include average
cladding temperature less than 1200°C (roughly 2200°F) during a LOCA for BWRs and PWRs
and no incipient melting of the fuel at centerline temperature during normal operation. The
typical operating temperatures of BWRs and PWRs are in the vicinity of 300°C. This is
significantly lower than the melting point of Zircaloy 2, seen in Table 1.2.
Table 1.2: Thermal properties of Zircaloy 2 (a phase) [1.13].
Property
Zircaloy 2
Density (kg/m3)
65,000
Melting Point (C)
1850
Linear thermal expansion coefficient (/°C)
5.9 x 10-6
Thermal conductivity (W/m°C)
13 (400°C)
1.5. NRC Concerns
NRC limitations on fuel bumup extend beyond the concerns of oxide thickness of fuel
cladding. Among the additional concerns, two dominated this research: core component bowing
and cladding degradation. Both of these concerns have direct relation to shadow corrosion.
Core component bowing, and its associated hazards, were identified as a concern to the
NRC through an Information Notice in September of 1989 [1.15]. Initial causes were
determined to be from ineffective modeling and the increased oxidation of fuel rods near onceburned assemblies with highly exposed fuel channels [1.15]. Although alteration of licensing
17
limits and core design has occurred, successful modeling and mitigation of shadow corrosion
was developed in response to the bowing reported in 1989. However, in March of 2003, GE
reported that new data suggested shadow corrosion caused bowing in a channel near a control
rod blade [1.16].
Cladding degradation is the second readily noted affect of shadow corrosion. The NRC
limits the predicted fuel rod oxidation in order to increase the reliability of fuel cladding integrity
during accident scenarios. The limitation on acceptance criteria, in accordance with 10 CFR
50.46(b) is that the maximum total oxidation of the cladding is not to exceed 0.17 times the total
thickness of the cladding before oxidation. The intent of this limitation is to reduce the
expectation of brittle fracture, and subsequent rupture, of fuel cladding due to the alterations in
the cladding properties. Since it has been noted that both irradiation time and temperature
influence oxidation, the study of shadow corrosion easily lends itself to investigation of
proposals to alter existing NRC criteria.
1.6. Past Developmentsin Understandingthe Shadow CorrosionPhenomena
An initial characteristic observed regarding shadow corrosion is the dependence of the
phenomenon on irradiation. The predictability of Zircaloy thickness changes when the sample is
exposed to a radiation environment. Early explanations identified the possibility that the
activation of materials, inducing increased P radiation, enhanced the oxide growth in the form of
shadow corrosion. However, experimentation conducted at MIT concluded that this was not the
instrumental factor, but indicated a strong electrochemical component to the phenomenon [ 1.17].
Despite the indications of an electrochemical aspect of shadow corrosion, difficulties in
replication of the phenomenon ex-core through experimentation indicated additional variables
were at play [1.18]. Since the elimination of the I5radiation hypothesis, tests at Halden and
18
Studvik have further examined the criteria for shadow corrosion. The Halden test reactor
performed two testing cycles, one in 1998 and the other in 1999, designed to test the effects of
spacers and geometry on shadow corrosion. The results of the Halden and MIT tests
demonstrated the inverse proportionality of distance between the "shadowing" component and
the Zircaloy to oxide thickness [1.18].
Also demonstrated in these tests was the electrochemical effect, which appears to be a
galvanic couple augmented by irradiation damage to the oxide layer enhancing the growth rate
and possibly electron transport assistance from y radiation [1.19]. The latest experimentation
from Studvik offers continued support for galvanic corrosion, with two notable discrepancies
[ 1.19]. The first discrepancy is that there is no apparent coupling device for Zircaloy and other
materials in-core. The second discrepancy is that there is no increased corrosion when Zircaloy
is coupled to a dissimilar metal in ex-core experimentation. Through experimentation with
electrically isolated samples using sapphire, the galvanic corrosion aspect of shadow corrosion
was suppressed. The same experiment also provided support for the theory that
photoconductivity, a form of electromagnetic radiation effect, participates in the phenomenon
[1.19].
1. 7.
NRC Documentation
As previously stated, the NRC has identified the issue of shadow corrosion as a factor in
the limitation of the allowable burn-up of fuel due to the uncertainty in oxide thickness. In noniradiated environments, zirconium and its alloys form a protective oxide layer that serves as an
effective barrier to corrosion. This oxide layer serves as an electrical insulator that prohibits the
transfer of electrons from the metallic matrix into the aqueous medium, while prohibiting the
adsorption of oxygen to the surface limiting continued oxide formation. In non-irradiated
19
environments, the limitation on observed, effective ion transport from the primary metal matrix
through the oxide to the aqueous solution occurs at approximately two nm [1.20].
The primary characteristic of the oxide that creates this limitation is the susceptibility to
spalling. However, the first action by the NRC found in the precursor research for this report
came in the form of an Information Notice issued in September 1989 [1.21]. In the Notice 89-69
(Loss of Thermal Margin Caused by Channel Box Bow), initial causes cited included inaccurate
modeling and estimates of the minimum critical power ratio. However, in August of 2003, the
NRC issued a supplement to the original finding stating that although alterations in modeling and
analysis, initial manufacturing of fuel and cladding, and differential irradiation growth mitigated
channel box bowing, shadow corrosion also induced the condition [1.15].
In compliance with 10 CFR 21.21(a)(1) GE Nuclear Energy (GENE) issued a
notification regarding the proof that shadow corrosion also contributes to fuel channel bow
[ 1.22]. Tied to the channel bow is the position of the control blade with respect to the channel
during the initial fuel cycle. The comments made in the report state that the fuel channel
experience absorbed hydrogen -induced growth of the channel wall closest to the control blade
resulting in bowing later in component life. The principal causes of the increased shadow
corrosion correlate to the criteria for galvanic corrosion: larger cathodic region when compared
to the anode and smaller gap between the control blade and the fuel assembly. In the case
reported, the BWR/6 lattice, noted to be afflicted by shadow corrosion-induced bowing, the
control blade is larger than blades characterized in modeling and the gap between the blade and
fuel assembly is uniquely smaller.
The findings observed in Studvik, Halden, and MIT experimentation, as well as the
observations from the GENE report, assisted in formation of a hypothesis for experimentation
20
and a related thesis.. The primary goal of the experimentation was to explore the possible
existence of galvanic current between Zircaloy and dissimilar metals in the irradiation
environment. This current is expected to result from alterations in the conductivity measured in
the coolant water and/or the materials themselves. Lastly, the final goal was an attempt to
measure the oxide characteristics through electrochemical impedance spectroscopy (EIS).
1.8. Thesis ProblemDescription
In order to support the galvanic current aspect of the hypothesis on the causes of shadow
corrosion, an electrochemical experiment measuring the potentials and currents between samples
of Pt, Zircaloy-2 (Zr-2), and Inconel (X-750) was conducted. The primary goals of this
experiment and subsequent thesis were to reinforce the findings of the evidence of the galvanic
couple dependency for shadow corrosion and the changes in the coolant due to radiolysis. In
order to accurately provide evidence of the galvanic couple, measurements of the reduction in
the conductivity of the high purity, low conductivity water used as coolant were conducted
through the use of a Pt-Pt electrode couple.
1.9. Outline of this thesis
In this chapter we introduced the concept of shadow corrosion, provided background on
the motivation for the research conducted, and presented the initial hypothesis.
Chapter 2 discusses the methodology and background of electrochemical analysis
including electrochemical potential and galvanic current measurement. Also included in this
chapter are the relation of these characteristics with respect to corrosion, means of measurement
available, and expected values from experimentation.
21
Chapter 3 discusses the experimental design. Included in this chapter are the
characteristics of MITR-2, MIT's research reactor, design of the assembly used in-core and excore, and supporting equipment. Incorporated with the supporting measurement equipment are
the computer codes used in the analysis and data collection.
The fourth chapter covers the results obtained from in-core and ex-core experimentation,
including obstacles encountered in experimentation. Chapter 5 conducts an analysis of the
results given in Chapter 4.
Finally, Chapter 6 gives the conclusions from the experimentation, including deviations
from expectations and recommendations for future work to further investigate the phenomenon
of shadow corrosion.
1.10. References
[1.1] Adams Atomic Engines, Inc., Protection for Fuel Elements: Ensuring Safety,
http://www.ans.neep.wisc.edu/-ans/point source/AEI/dec95/cladding.html, Atomic Energy
Insights, Volume 1, Issue 9, December 1995.
[1.2] Ramasubramanian, N., Shadow Corrosion, Journal of Nuclear Materials 328 (2004), pages
249-252.
[1.3] Zirconium in the Nuclear Industry, Proceedings of the 4th International Conference, held at
Stratford-upon-Avon, England, June 26-29, 1978, ASTM STP-681.
[1.4] Hixson, Robert S., George T. Gray, and Dennis B. Hayes, Shock Compression Techniques
for Developing Multiphase Equations of State,
http://www.fas.org/sgp/othergov/doe/lanl/pubs/las28/hixson.pdf, Los Alamos Science, Number
28, 2003.
22
111.5]
Sandvik Special Metals Corporation, Zirconium Alloy Fuel Clad Tubing: Engineering
Guide, First Edition, December 1989.
11.6]ASM International, Binary Alloy Phase Diagrams, Volume 3, 1990.
[1.7] International Nuclear Safety Center, "Zircaloy Heat Capacity,"
lttp://www.insc.anl. gov/matprop/zircaloy/zirccp/fmt html.pdi Nov. 13, 1997.
[ 1.8] O'Donnell, J. R., Design, Construction, and Commissioning of an In-core Materials Testing
Facility for Slow Strain Rate Testing, Ph. D. Thesis, Massachusetts Institute of Technology,
September 1994
[ 1.9] Cox, B., Some thoughts on the mechanisms of in-reactor corrosion of zirconium alloys,
Journal of Nuclear Materials, 336 (2005), pages 331-368.
[1.10] Gibbs, G. B. and R. Hales, The Influence of Metal Lattice Vacancies on the Oxidation of
High Temperature Materials, Corrosion Science, Volume 17, 1977.
[1.11] Chung, H. M. and T. F. Kassner, Cladding metallurgy and fracture behavior during
reactivity-initiated accidents at high burnup, Nuclear Engineering and Design, Volume 186,
Issue 3, December 1998.
[1.12] Nikulina, A. V., Shebaldov, P. V., Shishov, V. N., Peregud, M. M., Ageenkova, L. E.,
Rozhdestvenskii, V. V., Solonin, M. I., Bibilashvili, Yu. K., Lavrenyuk, P. I., Lositskii, A. F.,
Ganza, N. A., Kuz'menko, N. V., Kotrekhov, V. A., Shevnin, Yu. P., Markelov, V. A.,
"Zirconium-based alloy containing Nb, Fe, O, Si, Ni, and C for nuclear reactor core
components," US Patent Application, US6776957, 1999.
[1.13] Todreas, Neil E. and Mujid S. Kazimi, Nuclear Systems I: Thermal Hydraulic
Fundamentals, Hemisphere Publishing Corporation, 1990.
23
[1.14] NRC Meeting transcript, Briefing on High-Burnup Fuel Issues,
http://www.nrc.gov/reading-rm/doc-collections/commission/tr/1997/19970325a.html, March 25,
1997.
[1.15] NRC Information Notice 89-69, Loss of Thermal Margin Caused by Channel Box Bow,
http ://www.nrc.gov/reading-rm/doc-collections/gein-comm/info-notices/1989/in89069.html,
September 29, 1989.
[1.16] NRC Event Notification Report, http://www.nrc.gov/reading-rm/doc-collections/eventstatus/event/2003/20030609en.htnl,
June 9, 2003.
[1.17] Chatelain, Anthony R., Enhanced Corrosion of Zirconium-Base Alloys
in Proximity to Other Metals: the "Shadow Effect", S.M. Thesis, Massachusetts Institute of
Technology, MA, February 2000.
[1.18] Andersson, B., M. Limbick, G. Wikmark, E. Hauso, T. Johnsen, R.G. Ballinger, and A.-
C. Nystrand, Test Reactor Studies of the Shadow Corrosion Phenomenon, Zirconium in the
Nuclear Industry: Thirteenth Symposium, pages 583-613.
[1.19] Lysell, Gunnar, Ann-Charlotte Nystrand, and Mats Ullberg, Shadow Corrosion
Mechanism of Zircaloy, ASTM, 2002.
[1.20] Cox, B., Mechanisms of Zirconium Alloy Corrosion in Nuclear Reactors, The Journal of
Corrosion Science and Engineering, Vol.6, paper 14, 2003.
[1.21] NRC Information Notice 89-69: Loss of Thermal Margin Caused by Channel Box Bow,
Septermber 29, 1989.
[1.22] GENE report, Part 21 Notification: Fuel Channel Bow Reportable Condition and 60-Day
Interim Notification, MFN 03-012, March 3, 2003.
24
2. Electrochemical Analysis
Electrochemical measurements of dissimilar metal couples in aqueous solutions are a
means of understanding the rate and characteristics of observed corrosion phenomena.
Measurements to characterize the corrosion observed are either direct current or alternating
current, depending on the information desired about the electrode/electrolyte system. Direct
current measurements include electrochemical potential- and galvanic current-based. Alternating
current measurements are commonly referred to as electrochemical impedance spectroscopy
(EIS). EIS enables creation of equivalent circuits that mimic observed characteristics of the
electrode internal resistivity, electrolyte conductivity, and associated Helmholtz double layers
created by adsorption of electrolyte onto the surface of the electrodes. Using models developed
from EIS, the nature of the oxide layer (thickness, conductivity, etc.) can be obtained.
2.1. ElectrochemicalPotential
As dissimilar metallic electrodes are placed in contact, either directly or through an
aqueous solution, there is a transfer of electrons as the electrodes take on the role of cathode or
anode. As the oxidation and reduction reactions occur, a galvanic cell is developed. The
electrons on the anode are released from the metallic matrix as the ions are released into the
aqueous solution in the initial half-cell reaction. The second half-cell reaction, taking place on
the cathode, removes the more noble ions from the solution and returns them, along with free
electrons to the cathodic electrode.
The rate of the respective half-cell reactions creates a current differential between the
electrodes due to the flow of electrons. The current correlates to a voltage based on the
resistance inherent to the components in the electrode system. This voltage between the cathode
and anode, when no current is present, is commonly referred to as the corrosion potential. The
magnitude of the cell voltage varies dependent on the metals paired as the anode and cathode.
Experimental values have been measured for many of the commonly used values for standard
reduction potentials of many elements, often with respect to the standard hydrogen electrode
(SHE) at 25°C, 1 M or 1 atm.
The necessity for specifying the reference temperature indicates that there is a strong
dependence on temperature for the potential. Also factoring into the potential are the
concentrations of the oxidized and reduced species in their respective half-cell reactions. The
expected reaction contributing to oxide formation on Zircaloy is seen below.
Zr + H20 -> ZrO2 + 2(1-X)H2 + 4xH
From this reaction, the potential develops and is modeled by the Nernst equation. From
experimentation conducted by Cox, the potential is approximately -1.1V at 3000 C and limited by
the electrochemical isolation created by the oxide layer [2.1]. Without radiation, the oxide layer
limits the migration of electrons from the metallic lattice effectively limiting corrosion.
However, the oxide layer in irradiation fields appears to demonstrate characteristics inconsistent
with the oxide formed without radiation and radiolysis products. The oxide that forms in the
irradiation environment demonstrates electrochemical characteristics similar to porous oxides.
This enables easier transport of electrons to the aqueous solution, leading to linear growth of
oxide thickness [2.1].
2.2. GalvanicCurrent
The current measures the flow of electrons from one material to the other through the
electrodes as the pair acts as an anode/cathode system. In this system, the corrosion rate of each
electrode shifts in response to the relative electrochemical nobility of the electrode. The noble
26
electrode performs the role of the cathode, where reduction takes place. The anode, conversely,
experiences an increase in corrosion rate.
Also affecting the corrosion rate of the anode/cathode couple is the ratio of surface areas.
Ideally, it is desirable for a significantly larger anodic surface area when compared to the
cathodic surface area. For the experiment conducted in this thesis research, the surface area ratio
used was 1:1.
However, in addition to the surface area ratio and relative potential of each of the
samples, temperature and pressure, along with the composition of the aqueous solution, affect the
couple. In reactor studies, particularly those in BWRs, the coolant chemistry appears to
dominate the response of the system. The characteristics of the coolant in the BWR lead to
expectations that the aqueous solution used, high purity, low conductivity water, should serve as
electrical insulation of the materials, thus preventing the galvanic couple from forming.
However, through radiolysis, the inclusion of species, such as eaq', H+ , H, OH, O, HO 2, H 2, and
11202,
alters the expected conductivity of the electrolyte. This alteration should be evident
through the changes in conductivity.
2.3. Alternating Current Impedance
In many materials, using alternating current measurements of the changes in potential of
corroding material reduces the effect of induced polarization or passivity experienced with direct
current measurements [2.2]. The ability to measure near-actual potential values led to
experiments measuring and hypothesizing about corrosion of materials based on electrolyte
concentration and electrochemical characteristics of the surface of the corroding material. As a
foundation of alternating current use in corrosion analysis, Warburg, in the late nineteenth
century, determined that changes occur in the concentration of the oxidizing and reduced
27
materials with periodic regularity, corresponding to the alternation of the applied current [2.2].
Using this determination, Warburg hypothesized that the changes in concentration acted as an
electrical circuit composed of a resistance and capacitance. This modeling of the
electrochemical behavior of the corroding material is commonly used in development and
understanding of corrosion behavior today.
Despite the desire to use EIS to observe in situ corrosion, observations illustrate that the
alternating current used can alter the corrosion phenomena resulting in a shift in the polarization
curves in active/passive metals, effectively removing the passive region [2.2]. Experiments
investigating the shift in the polarization curves determined uncompensated ohmic drop (UOP)
removed the passivity region in active/passive metals [2.3]. Other observations of the affects of
EIS include increased corrosion in materials, dependent on exposure environment, e.g.
electronegative metals in soil [2.2]. However, despite the observations of changes in behavior
for specific materials and environments, EIS methodology evolved with procedures
compensating for unwanted interactions and affects allowing determinations of the in situ
behavior of many materials, enabling increased understanding of the kinetics of corrosion
reactions through development of equivalent circuits. These circuits can then be used to perform
elapsed time evaluations of corrosion or other virtual experiments matching the original
compositions of electrode/electrolyte system measured using EIS. As many corrosion
experiments are difficult to reproduce exactly, the ability to create equivalent electrical circuits
allows modeling and calculations of expected corrosion behavior in different environments.
EIS is commonly used to measure general corrosion rates in terms of equivalent circuits,
attributing capacitance to the Helmholtz double layer and resistance to the layer of oxide or
corrosion products on the surface of the corroding material. Using corrosion monitoring devises,
28
such as frequency or impedance response analyzers, potentiostatic or galvanostatic controllers,
and various computer programs, the measured impedance allows determination of a simple
circuit to resemble the material. However, several possible circuits can model the same
measured impedance. Further testing is required, along with regression-type analysis, to
determine the circuit best representing the measured corrosion process for a given material. One
plot commonly used in EIS is the Nyquist plot, seen in Figure 2. 1, which measures imaginary vs.
real impedance. This division enables identification of three primary values: polarization
resistance (Rp), uncompensated resistance (Ru), and maximum phase angle (Omax). Rp is the
overvoltage of the system at zero current density and Ru is the resistance of the oxide layer.
N
H
F__
Z Real
-
.
Kp
Figure 2.1 Ideal Nyquist Plot
Using the Nyquist Plot, Rp and Ru are calculated from the intersections of the plot with
the real axis and the capacitance of the double layer (Cdl)calculated from the maximum point of
the plot with respect to the imaginary axis (max) give the basic, expected equivalent circuit. One
of the advantages of EIS is that knowledge of the exact relationship between activation
29
polarization and the rate of reaction represented by current density, commonly referred to as the
Tafel slope, for the anode and cathodes is not required. This is because the changes in the
corrosion rate affecting Rp are beyond the normal range of values in most electrochemical
systems [2.4]. Another advantage is the ability to compute Cdldirectly from the Nyquist Plot.
This is possible from taking the inverse of the product of Rp and Omax.A second plotting method
used frequently in EIS is the Bode Plot method, seen below.
LIZI
-
Log
()
(Frquency)
a
e
(PhaseAngle)
Log (u)
(Frquency)
b
FIGURE7 - (a) and (b): Bode type of plots of
circuit in Figure 6.
Figure 2.2 Ideal Bode Plots
The two Bode Plot types consistently used from the Bode Plot method are the Bode
Magnitude Plot and the Bode Phase Plot. As seen in Figure 2.2, the upper plot is the Bode
Magnitude Plot, a log-log plot of the absolute value of impedance vs. frequency. The lower plot
in Figure 2.2 is the Bode Phase Plot, a semi-log plot of phase angle vs. frequency. Using the
Bode Plot method to find the equivalent Cdlis also possible. Using the Bode Phase Plot,
,,max
found corresponds to the frequency where the magnitude of the phase angle is of greatest value.
30
(It is important to mention that the value of w0maxin the Bode Phase Plot usually does not match
the value from the Nyquist Plot.) The equation, from Kelly, et al, to calculate Cdlfrom Bode
Plots is [2.4]:
Cdl = (max
*Rp)-l(1 + Rp/Rs)/
12
Both the Bode Plots and Nyquist Plot created from EIS software, potentiostat, and frequency
response analyzers allow for the creation of the equivalent circuit representing the electrical
analog of the corroding material.
2.4. References
[2.1] Cox, B., Mechanisms of Zirconium Alloy Corrosion in Nuclear Reactors, The Journal of
Corrosion Science and Engineering, Vol.6, paper 14, 2003.
[2.2] Venkatesh, S. and Der-Tau Chin, "The Alternating Current Electrode Processes", Israel
Journal of Chemistry, Vol. 18, pages 56-64, 1979.
[2.3] Mansfeld, Florian, "The Effect of Uncompensated Resistance on the True Scan Rate in
Potentiodynamic Experiments", NACE - Corrosion, Vol. 38, No. 10, pages 556-559, October
1982.
[2.4] Kelly, Robert G., John R. Scully, David W. Shoesmith, and Rudolph Buchheit,
Electrochemical Techniques in Corrosion Science and Engineering, Marcel Dekker, Inc., New
York, 2003.
31
3. Experimental Design
The main means of measurement of electrochemical properties involves placing samples
of the metal or metal alloy to be characterized in a conductive solution, either aqueous or
polymer, and measuring the potential and current between one of the samples to a second
sample. Each of the samples is called an electrode, with the electrode to be measured dubbed the
working electrode. Common experimental practices utilize a three-electrode system. In the
standard three-electrode system, the electrode paired with an electrode called the counter
electrode. The third electrode is the standard electrode, or reference electrode, and is used to
provide a basis for the measurement.
The standard means of measuring the electrochemical potential is determining the
difference in the voltage produced with respect to a reference. Commonly used reference
electrodes, in a three-electrode system include the standard hydrogen electrode, standard
silver/silver chloride electrode and standard calomel electrode. Since current was the primary
variable desired, not potential, a two-electrode system was used in this work.
A two-electrode system only measures the voltage produced between the working and
counter electrodes, without a reference. In order to determine the contribution of each electrode
to the overall cell voltage, a series of two electrode measurements conducted between
Zircaloy/X750, X750/Pt, and Zircaloy/Pt give the opportunity to determine the true
electrochemical nature of the oxidation reaction in the irradiation environment. A final Pt/Pt
electrode system was used to measure the conductivity of the electrolyte. In this experiment, this
electrode should provide support (or non-support) of the hypothesis that the radiolysis process
sufficiently alters the conductivity of the water to induce a galvanic couple between Zircaloy
cladding and dissimilar metals.
In order to determine the changes in the galvanic current and the conductivity of the
water, measurements were conducted using a specially designed assembly in the MIT reactor in
two primary conditions: zero power and approximately 4 MW power. The zero power readings
offered baseline galvanic current and potential values used to determine trends based on time and
power. Additional "spot" measurements were made at 1 through 3 MW.
3.1. Design of the ElectrochemicalMeasurementAssembly and Experiment
Figure 3.1 illustrates the arrangement of the samples selected for analysis that included
Zircaloy 2 (Zr-2), a Ni-based alloy (X-750), commonly used as a structural material within the
reactor core area, and Pt, known to be more noble when compared to the two alloyed materials.
The sample sizes allowed for uniform exposure area of 7 cm2 for each material respective to the
other samples inside the experimental assembly. The constant exposure area normalizes the
electrochemical values due equal area of the cathode and anode for adsorption of the electrolyte
constituents for reaction.
X-750
Zr-2
Pt
Pt
Figure 3.1: Top down view of specimen arrangement in module [3.1]
33
Uniform spacing of each sample at 0.7 mm and electrical isolation of the Zr-2, X-750,
and Pt samples was controlled by spacers made of plastic for laboratory bench testing and
alumina for autoclave and reactor testing. The size of the samples and the uniform spacing
enabled a cell constant of 0.01/cm, matching a conductivity cell used in conjunction with the
conductivity meter. This isolation leaves the possibility of the galvanic couple determined
completely by the aqueous medium and its properties. The high purity water expected in the
reactor and ex-core testing has sufficiently high resistivity contributing to the theoretical
electrical isolation of the samples. However, the radiolysis products produced during irradiation
are hypothesized to lower the conductivity of the water enabling the galvanic couple to occur.
The experiment required two stages of data collection: ex-core and in-core. The ex-core
experimentation included bench and autoclave testing with an assembly resembling the one
inserted into MITR-2. The primary difference between the assembly inserted into MITR-2 and
the configuration used in the laboratory testing was the omission of the flow shielding placed
around the assembly placed in the reactor to direct the flow along the length of the samples, seen
in Figure 3.2. The flow shield was omitted in the autoclave experimentation in order to allow the
water around the samples to freely communicate with the bulk solution.
The experimental set-up required the ability to control the flow through the experiment,
ensuring near equivalency in the flow rates at each face of the specimens. The shroud used to
control the flow patterns, along with the flow channel, is seen in the side view of the
experimental assembly, Figure 3.2. Also seen in this diagram are the coaxial leads used to
connect the specimens with the monitoring equipment in order to measure the electrochemical
data during the insertion into the autoclave or reactor core.
34
Flow Channel
Autoclave
Snecimen Cage
hmroud
Coaxial leads
3.9 mm dia.
8 mm
40 mm
10mm
Figure 3.2: Side view of specimen arrangement in module [3.1]
In order to minimize the contribution of the connections to the overall cell potential, the
connectors were plated with Ni. The Ni-plated end of the connectors was spot welded to the
electrode. After spot welding was completed, the welded ends were covered with 0.001
thickness stainless steel shim material to reinforce the weld. The area covered was 0.5 mm 2 on
each side of the sample.
The coaxial connections were then welded into a 0. 16-inch diameter Ti tube. The
connection wire was sheathed in insulation to prevent shorting of the connection to the sample
with the individual tubing. The four individual sample wire protection tubes were then inserted
into a larger Ti sheath that was welded to the end of the experimental assembly. The large tube
was then inserted into the reactor core with the individual sample connections attached to
shielded coaxial leads and cords. The coaxial cords were the primary connections to the
electrochemical measuring equipment.
35
3.1.1. Electrochemical Measurement Equipment
There were four primary pieces of electrochemical equipment used in the course of this
experiment: Solartron 1250 Frequency Response Analyser, Solartron 1286 Electrochemical
Interface, Keithley Model 617 Programmable Electrometer, and Thornton 200CRS
Conductivity/Resistivity
Instrument. In addition to the electrochemical equipment, a HP 3488A
Switch/Control Unit and IBM ThinkPad® 760CD were used to control and record the
experimental data gathering. The required connections between the electrochemical equipment
are seen in Figure 3.3. The numbers on the multiplexer correspond to the available ports on the
circuit card, four of the eight ports were used, two per output channel. The Solartron 1286 has
four input ports used for electrochemical measurements. Reference 1 and 2 (RE and RE2) are
provided for three- and four-electrode systems, where a reference electrode is used in
measurements. In two-electrode configurations, RE1 is shorted to the working electrode and
RE2 is shorted to the counter electrode, also seen in Figure 3.3.
36
Figure 3.3: Electrochemical monitoring equipment arrangement
I
l
P model 3488
multiplexer
14~~fl
Solartron
SolaJrtron
1286
-
I
0
I1
-750
°:
F
lPtP
.
1
.
I
I
I
I
_
I
3:Pt
_
_
_
_
2
I
3
COM
I
0
COM
I
1
_
2L:i IIZ
_~
RE1
I
2
3
-_a
Computer
WE
CE
RE2
i
T1-
The Solartron 1286 is designed to measure DC electrochemical properties of electrodes,
in two-, three-, or four-electrode configurations. For each electrode configuration, two values
are measured: the voltage differential and the current between the working and counter
electrodes. The current is defined as positive when current measured flows out of the working
electrode and into the counter electrode.
The Solartron 1250 measures the gain and phase characteristics of the electrode couple
tested. The primary controlling mechanism is the ZPlot® software loaded onto the ThinkPad®,
which issued the commands to the equipment and gathered the returned data. The primary
function of the Solartron 1250 is to use alternating current to gather electrochemical data with
minimal disruption to the electrodes and their properties. There are three main sections of the
Solartron 1250: an electrical stimulus generator, which produces a sinusoidal, square, or
37
triangular waveform, and two analyzers, one conducting single point measurements and the other
conducting point-to-point measurements.
The Keithley 617 was used to verify the readings obtained from the Pt-Pt couple in the
reactor core. The measurements obtained from the Keithley 617 were of conductivity, and in the
constant current mode. Also used to measure the resistance in the Pt-Pt couple was the Thornton
200CRS. However, the Thornton meter experienced failure during the in-core experimentation
warranting replacement of the unit with the Keithley 617. Initial ex-core bench testing was
conducted using the Thornton meter with later ex-core testing conducted with the Keithley 617.
3.2. ComputerPrograms
In order to ensure proper entry of commands into the electrochemical equipment, a
routine in Visual Basic® controlled the switching unit, Solartron 1286 and 1260. This routine
created an Excel® workbook containing individual worksheets for each of the tested couples: X750/Pt, X-750/Zr, Zr/Pt, and Pt/Pt. For each worksheet used, the routine gathered the potential
and galvanic current data by controlling the Solartron 1286. The routine also possessed an
embedded algorithm to control an alternating current impedance measurement program, ZPlot®.
ZPlot® issues commands to the Solartron equipment and records the returned data to
determine alternating current impedance. The results returned are displayed in the associated
program, ZView®. The data can be represented as either a Bode or Nyquist plots. From these
plots, equivalent circuits for the oxide film, base metal, and electrolyte may be produced.
The data gathered from the electrochemical equipment was sent directly into workbooks
created for each session of data collection. In this format, the ZPlot® data was extracted. The
Zplot® data then was entered into the comma-separated variable format and edited using
38
'Wordpad®. After editing, the format was readable using ZView® and could be used to create
associated Nyquist and Bode plots.
3.3. Experimentation in LaboratoryEnvironment
There were two phases to the ex-core experimentation, one completed using a bench
assembly and the second in an autoclave in reactor. The bench assembly was used primarily to
test the Pt-Pt conductivity measurement correlation to the measurements observed using the
Thornton conductivity meter. A second motivation to the bench testing was to ensure that the
Visual Basic® programs to control the experimental equipment performed the necessary
measurements. The initial phase of laboratory experimentation was conducted with a replica
assembly with plastic spacers instead of the alumina ceramic spacers. The substitution was made
because the environment in which the testing was conducted did not require the resiliency of
ceramic. The testing on the bench was conducted first in an open beaker, due to the desire to test
the operability of the program. Later testing was conducted in enclosed electrochemical
experimentation glass flasks that enabled entry of the experimental assembly, the probe for the
Thornton conductivity meter, direct feed of high-purity, low conductivity water into the flask. In
order to vary the conductivity of the aqueous solution, potassium chloride was used.
For the second phase of ex-core experimentation, the aqueous solution used was high
purity, low conductivity water. In order to preserve the desired qualities of the water, the water
was sent directly to the experimental set-up from the purifier via plastic tubing. The conductivity
of the water was measured in situ, in addition to the conductivity measurements obtained from
the Pt-Pt couple. Due to prior potential contamination of the system, an in-line single filter
system was placed downstream of the autoclave and was used to purify the system water to
resistivity levels near 15MD2/cm.Two electric heaters were wrapped around the exterior of the
39
autoclave enabling the water temperatures to be raised to 3000 C, at 1500 psi for non-irradiated
readings of environments comparable to BWR operating conditions.
3.4. MITR-2 Characteristics
The in-core experimentation was designed as a closed-loop system. This design, herein
after referred to as a "loop," enables control of the water chemistry and temperature without
significantly altering the operation of MITR-2, MIT's research reactor. The primary
experimental loop was inserted through the top of the reactor via one of the three ports used for
experimentation, seen in Figure 3.4. The MITR-2 is a light water cooled PWR reflected by
heavy water. The following descriptions illustrate the individual components of the
experimental loop set-up, which strongly resembled the ABB experimentation conducted by
Chatelain, containing the experimental assembly containing the four specimens of Zr-2, X-750,
and Pt [3.2].
Figure 3.4 Reactor Top [3.2]
The water chemistry and temperature of the water flowing past the specimens was
intended to resemble the environment experienced inside a BWR. The focus of this water
40
chemistry is the oxygen and hydrogen water chemistry used in BWRs to attempt to control the
affects of the radiolysis products, hypothesized to be a leading contributor to shadow corrosion.
Additionally, the water conductivity in the letdown system was monitored to determine the
alterations seen ex-core due to longer-lived radiolysis products, such as H202 . The main loop
contained a heating unit, comprised of a molten lead bath and recirculation pump to ensure
adequate flow rate through the experimental assembly.
Reactor coolant water flows down the external surface of the experimental assembly at a
flow rate of approximately 20L/min. After it reaches the bottom of the thimble, it enters the
experimental assembly, crosses the samples, and returns to the heater and recirculation pump.
There is a small portion of the overall experimental loop that is redirected after exposure to the
samples to monitoring equipment in the letdown system. It is this portion of the flow, assumed
to be representative of the bulk solution, that is measured for dissolved H2, dissolved 02, and
overall conductivity. The water flow path through the main loop is seen in Figure 3.5 [3.2].
Two principal components of the in-core assembly are the autoclave and thimble. The
autoclave is a 4.572 m long (grade 9) titanium tube running from the bottom to the top of the
reactor. The autoclave diameter is 3.175 cm. The main function is to serve as a pressure barrier
for the high-pressure high-temperature water and external environment. It also removes the
nuclear heating from the in-core section [3.3]. The thimble is outside the autoclave and is made
of A16061-T6, an aluminum alloy. It is the only component of the experimental assembly in
direct contact with the reactor coolant. It is designed to serve as an insulating boundary due to
the CO2 gas purge inside the thimble. The operational temperature of MITR-2 reactor coolant is
50°C, and exposure of the coolant to the temperatures in the experimental assembly adversely
affects the reactivity in-core.
41
ChargingFlow
Figure 3.5 Coolant Flow through Rig (Note: Not to scale)
To minimize the radiation dose emitted by the letdown system, including the heater and
recirculation pump, a covering of 5 cm layer of lead sheet, supported on a steel frame, along with
lead bricks were installed on the reactor top. There is also additional tubing leading to the pump
from the exit flow of loop water from the reactor top to allow for decay of short-lived isotopes,
such as N-16 to further reduced the emitted radiation. The shielding and pump are seen in Figure
3.6.
42
Figure 3.6 Letdown system from experimental assembly to recirculation pump [3.1]
The letdown system monitoring equipment was located on a raised platform adjacent to
the top of the reactor with the computer used to log the data from Labview(.
This data included
automated gathering of temperature, flow rate, and dissolved H2 and 02 from the letdown
system. Figure 3.7 gives depiction of the assembly and the charging system associated with the
letdown system. The letdown tank served to regulate the atmosphere experienced by the
experimental assembly.
43
Figure 3.7 Charging tank, letdown monitoring equipment, and chemistry control area
The water temperature across the specimens is controlled to simulate the expected
operational temperatures in BWRs. The temperature relay is set to regulate the temperature at
288°C. Temperature of the loop is monitored near the samples through a thermocouple inserted
into the assembly and at the heater outlet. The pressure for the assembly is set at 1500 psi to
prevent boiling of the water and control the density of the water exposed to the samples. Lower
density water would minimize the ability of the aqueous solution to serve as an electrolyte to
complete the galvanic couple.
The heater in the loop assembly automatically shuts off and must be manually reset if one
of the following eight conditions exists:
1. Loop water temperature near samples exceeds 290 0 C.
2. Loop water temperature falls near samples below 260 0 C.
44
3. Loop water temperature at heater outlet exceeds 295°C.
4. Heater lead bath temperature exceeding 370°C.
5. Main loop pressure exceeding 1500psi.
6. Main loop pressure falls below 1200psi.
7. Low charging tank water level.
8. Low auxiliary cooling water flow.
The justification for the actuation of the safety shutdown is to minimize the impact of ruptures in
the tubing associated with the loop or loss of electrolyte into the thimble.
The heater used to heat the leadbath is comprised of twelve strip heaters that surround
two stainless steel tubes. These tubes contain the letdown electrolyte and serve as a heat conduit
enabling the transfer of heat from the leadbath to the water prior to reentry into the reactor.
3.5.
References
[3.1] Peter Stahle, 2004.
[3.2] Chatelain, Anthony R., Enhanced Corrosion of Zirconium-Base Alloys
in Proximity to Other Metals: the "Shadow Effect", S.M. Thesis, Massachusetts Institute of
Technology, MA, February 2000.
[3.3] MIT Design Report, Enhanced Corrosion of Zirconium-Base Alloys in Proximity to Other
Material: "The Shadow Effect", December 3, 1998.
45
4. Experimental Results and Discussion
In evaluation of the collected data, the couples between Pt and Zircaloy-2, Zircaloy-2 and
X750, and Pt with Pt were expected to provide the significant insight into the corrosion process.
Appendices A through D present the time value graphs of electrochemical measurements.
4.1.
Galvanic Current Data Gathered
Figure 4.1 shows a plot of galvanic current v. power. Figure 4.1 illustrates that the
current increases with reactor power. This supports the hypothesis of increased coupling due to
the alterations in oxide properties and radiolysis products. However, there appears to be a
threshold power above which the current increases.
Figure 4.1 Galvanic Current V. Reactor Power
- ----- r
.....
U.
UUU
..
-
0.0002
7··~
7
~~:r·-··i·-··
C 0.00015
Z
i
k·
,
o_, irie, · ··
2-111,11 W,-·
i~_-
:
·
W.
P
0.0001
0.00005
0 1
0
1
2
3
4
5
Power (MW)
* Zr-Pt Amps (A)
X750-Zr Amps (A)
Seen in Figure 4.2, the change in resistance of the Zircaloy is greatly affected by reactor
power. After reactor power increased to 4 MW, the resistance is observed to decrease at a higher
rate, seen by the solid line. The two highest resistivity readings occurred at the initial insertion
of the experimental assembly into the reactor with zero reactor power, as seen in Figure 4.2. The
slope of the change in resistance with respect to time appears to increase slightly after the reactor
reaches 4 MW power.
Figure 4.2 Zircaloy-2 Resistance V. Time in Reactor
.
-
E
E
. ^-
I. UUt- UD
1.00E+04
I1.00E+03
o O
"'
m'
4~~~~~~~~· 5
1.00E+02
O~~~~~~~
B
*'$ 1.00E+01
nnr"1
I. UUUV T
a)
4
M-
r
-·
-
0
10
20
--
30
I
50
60
Number of Days
Zero Power
i
40
4 MW
i~~~~~~~~~~~~~~
The measurements of the changes in the potential of the Zircaloy with respect to reactor
power relative to Pt indicate changes in the system resistivity. Previous experimentation
determined that without radiation effects, Zircaloy becomes increasingly noble due to the growth
of the protective oxide film [4.1]. As seen in Figure 4.3, the resistance to current flow of the
Zircaloy and associated oxide layer, when the calculated resistance of the water is removed, is
seen to decrease, and the rate of decrease is dependent on reactor power. This supports the
hypothesis by Cox that the oxide characteristics change due to the radiation effects, assuming
constant resistivity in the bulk Zircaloy matrix.
Comparing the resistivity of the Zirconium alloy to the X-750, the predominant
relationship is that the X-750 experiences a lower rate of decrease in resistance to current flow as
seen in Figure 4.3. This predominance supports the observation that shadow corrosion is related
primarily to changes in the Zircaloy, while still affected by changes in the dissimilar metal
couple system.
47
Figure 4.3 Resistivity Comparison between Zircaloy- 2 and X-750 at 4 MW
1.UUE+05
1.OOE+04
a
'
1.00E+03
1.00E+02
1.00E+01
1.00E+00
0
10
20
30
40
50
60
Number of Days
* Zr-2 Resistivity (/cm)
4.2.
* X-750 Resistivity (/cm)
Conductivity Data Gathered
The Pt-Pt couple gives the resistivity of the water based on the resistance, calculated by
Ohm's Law, from the voltage and current during the ECP measurement.
This value was also
obtained directly by connecting the couple to either the Keithley 617 or Thornton conductivity
meter. The expected characterization is that the resistivity would decrease, correspondingly,
conductivity would increase, with reactor power.
The measured results from the individual two-electrode system of coupled Pt-Pt
electrodes at 220 C and atmospheric pressure are seen below in Figure 4.4. In order to correlate
the data obtained in-core with an expected value ex-core, a best-fit line was created using the
following equation:
Pt-Pt value = 0.065964 (Thornton value)
Where all units are S/cm.
48
_
__
Conductivity Correlation
E .-- ,"I
,1
0.0002
I~~~~~
'"'
,0.01...
.- ,.
-. :
.',
:,
A
0.00015
0.0005
0
0
0.0005
0.001
0.0015
Thornton measurement
0.002
0.0025
0.003
(S/cm)
Figure 4.4 Pt-Pt correlation chart
This correlation indicates that there is a linear relationship between the measurements
conducted by the conductivity meter and the Pt-Pt couple. This validates the assumption that the
measurements conducted within the core will reflect the differences in conductivity measured by
the couple of Pt-Pt electrodes.
Analysis of the in-core data gathered starts with the basis of the experimental hypothesis;
radiolysis alters the chemical concentrations of the coolant, affecting the conductivity. This
hypothesis was tested using the potential values obtained from the Pt-Pt coupling of electrodes.
Appendix E illustrates the values of the Pt-Pt electrodes for potential and current measured,
Ohm's Law was used to calculate resistivity and conductivity at operating power. All
calculations of resistivity and conductivity acknowledge that flow of electrons determines the
sign of the values for voltage and current. Correspondingly, the absolute value for the resistivity
and conductivity is analyzed due to higher importance of the magnitude of the electron flow
impediment. Seen in Figure 4.5, the values obtained for conductivity at no reactor power are
49
scattered over a notably smaller, and lower, range than the values measured at 4 MW power.
This data also shows the apparent threshold effect observed in the current.
Figure 4.5 Coolant Conductivity, as measured by Pt-Pt electrode, V. Reactor Power
4AA.LA
I.VVr-
'
·~t
1.00E-01
t*t
1.00E-02
"o
0 "m ?
'
1.00E-03
1.00E-04
1.00E-05
1.00E-06
m
1.00E-07
1.00E-08
X
1.00E-09
1 nnF' in
Power (MW)
The measured values are plotted in Figure 4.5. While the data are scattered, the general
trend is an increase in the measured conductivity with increases in reactor power. This is
supported by the conductivity measurements obtained in the letdown system, seen in Figure 4.6.
50
Figure 4.6 Letdown Conductivity Measurement V. Reactor Power
Letdown Cond
9
-~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
8
i~
ii~:iill
~~ .
7
E
'=
0 6
7
He~~~~~~~~~~~~~~~~~;I
E.
i~~~~~~~~~
' ~
'
"~~~~~~~~~~~~~~~:·
· ·"
i
-~~~~~~~~~~~~
4
o
:3
·
2
~
·
-~~~~~~~~~~~~~~~~~~~~~~~~~~~
:'
v;·:
ii!
-
~ ~~~~~~~~~~~~~~~~~~~
· ,
,
,
Of
0
0.5
1
1.5
2
2.5
3
3.5
4
4.5
5
Power (MW)
The results support the initial hypothesis that reactor power alters the conductivity of the
high purity, low conductivity reactor coolant water via radiolysis. Also of note, is the relatively
constant value in the conductivity at 1, 2, and 3 MW power. This measurement suggests a 4
MW threshold of power, and associated neutron flux, required for notable changes in the
conductivity of the coolant. Observing the time dependence of change at 4 MW power illustrates
that the conductivity also increases with time at power, seen in Figure 4.7.
51
Figure 4.7 Coolant Conductivity, as measured by Pt-Pt electrode, V. Time at 4 MW Power
A
ffr-
.
I .UUr'rUU
ffl
1.OOE-01
1.OOE-02
E
1.00E-03
t
1.OOE-04
'~ 1.00E-05
0
1.00E-06
o
1.00E-07
1.OOE-08
1.OOE-09
1.OOE-10
Readings at 4MW
This observation indicates time-dependency, in addition to the observed power
dependency.
4.3.
Galvanic Current and Conductivity Analysis
The conductivity of the coolant and the galvanic current of the measured systems
increase with reactor power, Figures 4.8 and 4.9 indicate correlation at 4 MW between
conductivity measured by the Pt-Pt electrode and corresponding measurements of galvanic
current between pairings of Pt and Zr-2 and X-750 and Zr-2 electrodes, respectively.
52
I..
Figure 4.8 Zr-2-Pt Measured Galvanic Current V. Pt-Pt Measured Conductivity
I~~~~~
'~:--',,~:i{,,,,
...0.00008
,':,
,,,,' , I' ,
.0
-
0.00007- :
0.00006
0.00005
2
. ' . '~ .
.
,'1,I,,
r 0.00004
3[
0.00003
0.00002
IL 0.00001
---
......
0
0.OOE+0 2.00E0
07
N
4.00E07
6.00E07
8.00E07
1.00E06
1.20E06
Pt-Pt Measured Conductivity (S/cm)
Figure 4.9 Zr-2-X-750 Measured Galvanic Current V. Pt-Pt Measured Conductivity
0.00009-
r
Ž 0.00008
n
...
r:
0.00007
, 0.00006.
.
0.00005
m @0.00004
.
' . :
:
3 0.00003
=
_.Q
c-4
Nr
X
nm^n
u.uuuz0.00001
0.OOE+0 2.00E0
07
4.00E-
6.00E-
8.00E-
1.00E-
1.20E-
07
07
07
06
06
Pt-Pt Measured Conductivity (S/cm)
These findings support the hypothesized correlation between conductivity and galvanic
current.
4.4.
Obstacles Encounter During Experimentation
After installation of the experimental assembly into the reactor, there were several
deviations from the initial design of the experiment. Among the deviations, technical issues
53
arising from the Visual Basic® code written to gather the data caused the ThinkPad® to suspend
normal functioning during data collection or dump physical memory causing the data taken in
that session to be erased. Initial laboratory testing indicated minor flaws in the first Visual
Basic® program, a revision was completed prior to implementation in the reactor. This second
version was initially used in the in-core testing. After the installation, the program was further
tested and revised to assist with ease of data acquisition. However, the third version created
duplicates of the Pt-Pt couple data, overwriting the X750-Pt couple data, and left the data set
incomplete. The program was altered for a fourth time, and this program was used for the
duration of the experimentation.
Initial laboratory attempts to create the associated EIS plots indicated high levels of
electrical noise being gathered with the data. In order to minimize the noise in the data, the
connections from the end of the titanium tubes containing the wires connected the samples were
shielded using a specially designed brass connector. The connector screwed into the end of the
coaxial connector and covered the end of the titanium tube to reduce exposure to superfluous
fields that may induce the noted noise. Also noted to contribute to the noise was the coaxial
cables used to connect the samples to the electrochemical equipment. Using an oscilloscope, it
was noted that some of the wires created noise due to insufficient connections or shielding.
Along with the brass shields, replacing the faulty wires reduced the noise noticed in the
laboratory environment.
Despite the ability to reduce the noise in the laboratory environment, there remained
significant noise in the alternating current impedance data gathered in-core. When compared to
the ideal plots in chapter 2, the desired locations of the indicative points that are used in creation
of the equivalent circuits are unintelligible.
With the excessive electrical noise seen, there is no
54
ability to determine the corrosion rate and conductivity of the oxide forming on the zirconium
alloys.
There were also significant issues with controlling the expected water chemistry. Despite
the introduction of hydrogen through the charging tank, the levels of dissolved oxygen at 4 MW
remained significantly higher than the desired level. During experimentation, the levels of
dissolved oxygen exceeded the desired levels of 200 ppb, with nominal values ranging from 100
to over 500 ppb. Dissolved hydrogen measured in the letdown system also never reached the
desired level of 30 ppb. Average values of dissolved hydrogen in the let down system were
around 11 ppb during 4 MW operations. During the period of heater inoperability, the levels of
dissolved hydrogen and oxygen spikes, giving values of approximately 400 to 600 ppb for
hydrogen and 1.5 ppm for oxygen. The desired test conditions and measured conditions during
experimentation are seen in Table 4.1.
Table 4.1: Experimental Conditions
Desired Experimental
Conditions
Actual Experimental
Conditions
lemperature
280 0C (5200 F)
80°C (174°F) to 2800 C (520°F)
I)issolved Hydrogen
Dissolved Oxygen
30 ppb
200 ppb
11 ppb to 600 ppb
100 ppb to 1.5 ppm
The deviations from the desired values resulted from deficiencies in the primary
experimental loop, included malfunction of the leadbath heating unit. The malfunction was due
to a steam leak within the heater assembly leading to water being released onto the reactor top.
In addition to the issue of water leaking onto the top, there was the potential for steam etching on
surfaces contacted by the high-pressure steam leading to a larger rupture and further
contamination and/or damage. Evaluated data omitted the period of heater inoperability. While
the heater underwent repairs, the experiment remained in place, but the temperature dropped
55
from the expected regime of approximately 280°C (520°F) to 800 C (174°F). Even after repairs
were conducted, the temperature never exceeded 250°C (4800 F).
4.5.
References
[4.1] Cox, B., Mechanisms of Zirconium Alloy Corrosion in Nuclear Reactors, The Journal of
Corrosion Science and Engineering, Vol.6, paper 14, 2003.
56
5. Conclusions
The results of this research represent the first attempt to evaluate dynamic behavior,
including coupled current, potential and oxide character, of cladding and structural materials in
an actual reactor core at LWR operating temperature. The task was daunting and, although there
was an expectation of quantitative results, in the end due to the difficulties experienced, the
results were only semi-quantitative. Future experiments will benefit from the lessons learned in
this initial attempt.
5.1. Reiteration of Hypothesis
In order to evaluate the galvanic current aspect of the hypothesis on the causes of shadow
corrosion, an electrochemical experiment measuring the potentials and currents between samples
of Pt, Zircaloy-2, and Inconel (X-750) was conducted. The goal of this experiment was to seek
evidence of the galvanic couple dependency for shadow corrosion. In order to accurately
provide evidence of the galvanic couple, measurements of the reduction in the conductivity of
the high purity, low conductivity water used as coolant were conducted through the use of at PtPt electrode couple. Additionally, galvanic current measurements were made.
5;.2. Comparison of Experimental Results with Expected Results
The results of this research have shown that:
1.
Radiolysis increases the conductivity of the coolant to the point where
corrosion current may be possible between materials in close proximity.
2.
Current flows between Zircaloy-2 and structural materials in the in-core
environment.
Note: While current between Zircaloy-2 and structural materials has been identified,
further work and analysis is required to determine the exact nature of this current.
Sources of current could include redox current from water as well as corrosion current.
3.
There is an apparent threshold in reactor power - flux- above which current is
observed. One would expect that were the observed current due only to redox
effects, that there would be a linear relationship between flux and current.
4.
While the exact oxide composition changes related to the electrochemical
observations remains unknown, the indications that resistivity change in
Zircaloy, and its associated oxide, exist, as previously hypothesized by Cox,
giving a new avenue of exploration for the understanding of the shadow
corrosion hypothesis. Further metallurgical and compositional analysis of the
oxide film post-irradiation may result in better understanding of the root
causes of shadow corrosion.
58
Appendix A - Pt-Pt Couple Graphs
May 27, 2004 - first run, no power
GalvanicVolts
ECPVolts
0.006
0
-0.005
-0.01
9
1
0.005
0.004-
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,
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1 2 3 4 5 6 7 8 9 10
;
May 27, 2004 - second run, no power
ECPVolts
0
,
,
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"I
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Senesi1
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U
1
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,
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~~~~------
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.=..
May 28, 2004 - first run, no power
ECP Volts
0
1 :
-0.0
-0.02
-0.04
---
Seres
-0.05
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ECP Amps
Galvanic Amnps
-0.000026 ....
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May 28, 2004- second run, no power
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60
May 28, 2004 - third run, no power
__
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ECPVolts
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GalvanicVolts
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May 28, 2004 - fourth run, no power
ECPVolts
GalvanicVolts
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t
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June 4, 2004 - first run, no power
ECPVolts
GalvanicVolts
U
0 006
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i---- Series1
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.- .
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o
-- Sees1
0.02
-0.015
0.01
0
1
-0.02
2
3
4
ECP Amps
6
5
7
8
9
10
Galvanic Amps
0
0
1
-0.00001
-0.00002
-0.00003
9
1
-0.00001
I
:.:.:4.
5
6' :7
8'
8
1 0
-0.00002-
-Sees1
-0.00004
-0.00005
-0.00006
-0.00007
-0.00008
-0.00009
-0.00003
-
Senes1
-0.00004-0.00005
-0.00006
July 9, 2004 - 4 MW run
ECP Volts
13
1
-0 .0 02
17
-0.004
-0.006
-0.008
-- Se
-0.011
-0.012
_2
- 1U .
I 4r
M
.-
-
{
-
__
ECP Amps
-0.000056
3
5
7
I
I
9 .11
I
15
I
1
0.00004
0.00003
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3 '15 1
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iy I
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-0.00001
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e
-0.00003
-0.00004
-0.00005
-0.00006
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75
I
I :5 I
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1
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Galvanic Amps
I~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
July 12, 2004 - 4 MW run
ECPVolts
GalvanicVolts
-0.0064
0.07
-00068
0.06 0.05 -
-0.007
-0.0072
0.04
-0.0074;
--
0.03
Series
0.02 -
-0.0076
-0.0078
0 01
-0.008
-0E.0082
Amps
1
ECPAmps
2
3
4
5
6
7
8
9
10
GalvanicAmps
0
0
-0.00001
-0.00002
-0.00003
-0.00002
-0.0000oooo
-0.00004
---
Series1
-0.00005
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-0.00008
- -----
I~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
July 15, 2004 -4 MW run
GalvanicVolts
-0.0000
-0.00004
0.0000 GalvanicVoltAmps
0.040.06
-. 00003
ECPAmps
0
-0.00001
-0.00004
0.00006
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+Senes1
0.00008
a
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-- Senes1
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.
:'%/
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:
-000007
-0.00008
76
Appendix B - Zr-Pt Couple Graphs
May 27, 2004 - first run, no power
GalvanicVolts
ECPVolts
0.0045
0.004
0.0035
0.003
-0.29
-0.292
3
5
-0.294
-0.296
-"~
-0.298
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0.001
0.0005
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.
-0.308
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Series l
,
1
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2
3
4
5
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6
7
8
9
10
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0
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1
3
5
7
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0.0000160.000014
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-0.000015
0-0.00002
1
2
3
4
5
6
7
8
9
10
May 27, 2004 - second run, no power
ECPVolts
I'l
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1
t
3
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----
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---
7, -9
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y~~~~~~~~~
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GalvanicAnps
0
1
3
5
7
9
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1
0.000014
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0.00001
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0.000006
0.000004
0.000002
0
1
2
3
4
5
6
7
8
9
10
May 28, 2004 - first run, no power
ECPVolts
GalvanicVolts
0.003 -.
0
-
00025
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-
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0.002
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0.0015-
28,2004 - s nwne
Ma1
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r.
9
10
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0
1
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2
3
4
5
6
8
7
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ECPAmps
o
-0.00001
-0.00003
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-0.00004
-0.00006
GalvanicVolts
-0.000017
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S
0.006
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.
0.003
0.002
0.001
01
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ECPAmps
-0.000036
2
3
4
5
6
7
8
9
10
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0
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-.000038
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-0.00004
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-0.000008
-0.000044
-0.00001 -
-0.000046
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78
May 28, 2004 - third run, no power
ECP Volts
GalvanicVolts
-0.508
U.UU45
-0.51 1
3
5
7
0.004
II,
0.0035
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1
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0.0005
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1
2
3
4
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7
8
9
10
Galvanic Amps
0
1
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------
ECPAmps
-0.00001
5
13 15 47
0.00007
0.00006
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0.00005
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7
6
8
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10
May 28, 2004 - fourth run, no power
GalvanicVolts
ECPVolts
-0.488
,
;.1 I
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3
1.
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2
3
5
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6
7
8
9
10
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0.00006
0
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0
1
2
3
4
5
6
7
8
9
10
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June 3, 2004 run, no power
GalvanicVolts
ECPVolts
u
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i
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d;
-0.005
0.003
;
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r s.;
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Galvanic Amps
---Senesl
4
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June 4, 2004 - first run, no power
ECPVolts
,
-0.172
-0174 13
-0.176
-0.178
-0.182
-0.182
-0.188
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1
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4
5
8
9
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80
June 4, 2004 - second run, no power
GalvanicVolts
ECPVolts
-0.164
-0.166
-0.168
-0.17
n nn7
u.uU,
0.006
0.005
0.004
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\
4Senesi
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0.003
0.002
-0.174
-0.176
0.001
0
-0.178
1
-0.18
2
3
4
5
ECP Amps
6
7
8
9
10
9
10
Galvanic Amps
0.000006
0.000005
-0.00005
0.000004
-0.0001
--
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2
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3
,
4
5
6
7
8
June 4, 2004 -third run, no power
ECP Volts
GalvanicVolts
-0.208
0.006
-0.21
-
0.005
-0.212
-0.214
-0.216
0.004
0.003
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0
1
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2
3
4
5
6
7
8
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10
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ECPAmps
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0
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-0.00015
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0
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81
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5- a
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a
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June 4, 2004 - fourth run, no power
GalvanicVolts
* 0.0045
0.004
5
0.0035
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0.003
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0.0005
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0.000006
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0.00001
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ries
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June 4, 2004 - 1 MW run
ECPVolts
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0.000006
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-0.146
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3
4
5
6
7
8
9
10
Galvanic Amps
.- . 1 . ;
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82
.June4, 2004 - 2 MW run
ECPVolts
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-0.132
1
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0
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7
8
9
10
Galvanic Amps
.
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5
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1
3
4
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8
10
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June 4, 2004 - 3 MW run
ECPVolts
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June 4, 2004 - 4 MW run
.. 0.004
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5
6
7
8
9
10
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'
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June 7, 2004 run, no power
ECPVolts
GalvanicVolts
0.0014
0.0012
0
-0.02
0.001
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1
2
3
4
5
6
7
8
9
10
84
June 8, 2004- 4 MW run
ECP Volts
Galvanic Volts
0.0045
0.004
0.0035
0.003
0.0025
0
1
-0.01
5
'3
7
9
1
13
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0.002
0.0015
0.001
0.0005
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0
-0.06- II
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1
2
3
4
5
ECPAmps
6
7
8
9
10
GalvanicAmps
0
U.00005
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-0.000005 4
-0.000015
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3
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,
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June 9, 2004- 4 MW run
ECPVolts
Galvanic Volts
0.0035-
-0.064
0.003
-0.068
-0.068
-0.07
0.0025
0.002
-0.072
-0.074
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-0.076
-0.078
-0.08
-0.082
0.0015
0.001
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0.0005
0
1
2
3
4
5
ECP Amps
7
8
9
10
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0
1
3
6
7
9
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-0.000005
-0.00005
-0.001
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GalvanicAmps
0
1
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A
A
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?
-0.00001
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85
-e- Series1
L
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June 10, 2004 - 4.35 MW run
GalvanicVolts
ECP Volts
0.0018
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0.0016
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1
2
3
4
5
6
7
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8
10
9
ECPAnps
-0.00005
-0.0001
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Seesi
:..
-0.00015
June 11, 2004 - 4 MW run
-0.08
0 004
0.0035
0.003
0.0025
0.002
0.0015
0.001
0.00050
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-0.09
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i. .i:
GalvanicVolts
ECP Volts
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0
1
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6
2
3
4
5
6
7
8
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.
9
10
86
June 14, 2004 - 4 MW run
ECPVolts
0
Galvanic Volts
0.000045
0.00004
a .l:
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0.000025
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6
7
9
8
10
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0
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=_
June 15, 2004 - 4 MW run
ECPVolts
0
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-0.03
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i
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1
2
3
4
ECP Amps
5
8
6
7
8
9
10
GalvanicAmps
n nnnnnu-,u:
-U.UUUUU.U
-0.0000031
-0.00000315
-0.000005
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I--Seees1
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-0.00000345
iI
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--- Series1
June 16, 2004 - 4 MW run
ECP Volts
GalvanicVolts
0.00004
-0.02
-0.03
-0.04
0.000035
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0.000025-
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0.000015
0.00002
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v
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0.0000
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2
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4
ECPAmps
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-0.09
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Senes1
5
6
7
8
9
10
GalvanicAmps
.
-0.000003
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-0.000001
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-0.000002
-0.000003
-0.0000032
-00000025
-0.000003
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-0.0000035
-0.000004
-0.0000045
-0.000003
June 18, 2004 - 4 MW run
ECPVolts
Galvanic Volts
0.000045 -
-0.01
s
A
-0.02
4003
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0.000025
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0.0.000
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ECPAmps
GalvanicAmps
-0.0000031
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88
June 22, 2004 - 4 MW run
GalvanicVolts
ECPVolts
0.05-
0
-0.005
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0.02
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-0.035
-0.04
0
1
2
3
4
5
6
7
8
9
10
GalvanicAmps
ECP Amps
0
0
-0.0005
t
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June23, 2004 - 4 MW run
ECPVolts
GalvanicVolts
0
n n
u.vt
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7
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Seriesl|
I
0.03
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-0.08
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-0.1
2
3
4
5
ECPAmps
7
8
9
10
GalvanicAmps
-0.00001
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2
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4
6
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-0.00003
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June 24, 2004 - 4 MW run
ECPVolts
GalvanicVolts
0.05
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2
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5
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7
8
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-0.0002-0.0004
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-0.0008
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|
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-
-0.0012
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June 28, 2004 - 4 MW run
Series1
-.--
ECP AImps
GalvanicAmps
0
-0.000042
-0.000043
-0.00002
-0 00004
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-0.00008
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-0.000047
-0. 00049
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90
June29, 2004 - 4 MW run
GalvanicVolts
ECPVolts
U-
0.03,..U.Uj
0.025
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-0.5
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0.02
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1
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0.005
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0.015
0.01
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-I
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4- __
1
I
2
4
3
5
ECPAmps
1
3
5
7
9
7
8
9
10
8
9
10
-.
Galvanic Amps
0
-0.00001
6
0
11 13' 15 17 19
2
1
3
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5
4
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-0.00003
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SenesI
-0.00003
-0.00004
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June 30, 2004 - 4 MW run
GalvanicVolts
0.07
0.06
0.05- .
0.04
0.03 0.02
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0.01
0
-0.025
1
2
3
4
ECPAmps
7
6
8
9
10
9
10
GalvanicAmps
-0.000047
-0.000048 1
5
0
3
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11 13
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8
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91
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July 2, 2004 - 4 MW run
ECPVolts
GalvanicVolts
0
-0.00500
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0.05
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7
8
9
10
GalvanicAmps
-0.00001
-0.00002
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-0.00003
A004S
-0.00004
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-0.00005
-0.000062
-0.00006
July 6,2004
:,-.
|Se
:
4 MW run
GalvanicVolts
0.07
0.06
-0.00005
0.05
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-0.00001
-0.015
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1
ECPtAmps
-0.00002
3
4
5
6
7
8
9
10
GalvanicATps
0
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July 7, 2004 - 4 MW run
GalvanicVolts
ECPVolts
0.06
0
3
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T
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0.02
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0.04
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2 3 4 5 6 7 89 10
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3
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-0.00006
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July 9, 2004 - 4 MW run
GalvanicVolts
ECP Volts
0
-0.002
rn
U.u
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3
13 1'
:
7
0.05
-0.004
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0.04
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-0.008
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0.03
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0.02
0.01
0
-0.014
-0.016
1
2
3
4
5
ECP Amps
0
-0.00001
93
8
9
10
9
1J
0
a
1'
14' ..
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I3
4
-0.00002
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Galvanic Amps
-0.00002
-0.00004
-0.00005-0.00006
-0.00007.
6
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-0.00003
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,7 .6
|
July12, 2004-4 MW run
GalvanicVolts
ECPVolts
0.06
-0.0071
-0.0072-0.0073
0.05
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004
0
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July 15, 2004 - 4 MWrun
GalvanicVolts
ECPVolts
0.07
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|
400061
+
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;::;. L::;
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0.01
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4
5
6
7
8
9
10
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94
Appendix C - X750-Zr Couple Graphs
Mlay27, 2004 - first run, no power
Senes
GalvanicVolts
ECP Volts
-0.315
n nnr
-0.32 1
3
5
7
9
11
13 15
17
0.004
19
-0.325
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0.003
0.0025
0.002
0.0015
0.001
0.0005
0
E-
I
-0.345
1
2
3
4
ECP Amps
5
6
7
8
9
Senes1
10
Galvanic Amps
0
0.000012
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1
-
1
l ' "-17
.
1
0.00001
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0.000004
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1 2 34 5
May 27, 2004 - second run, no power
ECPVolts
-0.295
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-0.305
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i I
7
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3
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1i . . . .
13 15 .1
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t-.- Seriesi
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0.002
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0.0015
0.001
0.0005
0
1
2
3
4
5
ECP Amps
0
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-0.000004
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3
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5
7
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432
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6
7
9
10
Galvanic Amps
4.
I 4
0.000009
0.000008
0.000007
0.000006
0.000005
4-
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--- Sedesl1
A
.
0.000004-
-7-
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-
0.000003
0.000002
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1
1
1
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1
2
3
4
5
6
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95
8
7
8
9
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10
May 28, 2004 - first run, no power
ECPVolts
GalvanicVolts
;
0.004 .
-0.396
0.0045
-0,398
*
-0.4
0.0035
0.003
-0.402
0.002
Seies
-0.404
0.001
0.0005
0
-0.406
-0.408
1
-0.41
2
4
3
6
5
7
8
9
10
9
10
GalvanicAmps
ECPAmps
0.00004
-
0.000035
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0.000025
0.00002
0.000015
0.00001
-0.00002
+
0.000005
0
1
3
2
4
5
6
8
7
May 28, 2004 - second run, no power
GalvanicVolts
ECP Volts
-0.436
I3
-0.438-
0.0045
1
3f. :
I 9 1 119
$ 7
0.004
-0.440000
May28, 2004- second rn, no power
Sees
S
0.0035
0.0030.0025....
0.002
--
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0.0015
0.001
-0.444
0.0005-
-0.446
2
1
4
3
5
6
7
8
9
10
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0.000035
0.00003'
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0.000015.
0.00001
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0
1
2
3
4
5
6
7
8
9
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96
May 28, 2004 - third run, no power
GalvanicVolts
ECP Volts
0.0045
-0.522
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2
3
4
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5
7
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5
8
9
10
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2
3
4
5
6
7
May 28, 2004 - fourth run, no power
C(
GalvanicVolts
-0.516
0.0045
0.004
0.0035
0.003
0.0025
-0.518 1-3
-0.52
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0.001
5
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0.002
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1
2
3
4
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7
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5
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4
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0.000005
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-0.00007
97
1
2
3
4
5
6
7
8
9
10
June 3, 2004 run, no power
ECP Volts
-0.105
-0.11
-0.115
-0.12
Sees
-0.125
-0.13
-0.135
ECPAmps
Galvanic Amps
-0.0000066
0
-0.00000665
-0.00005
-- Seriesi
-0.0001
S
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gdts'
5
5
z
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-0.00015
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June 4, 2004 - first run, no power
ECP Volts
-0.178
-0.18, 1
S
. ,
-0.182
-0.184
|--
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-0188
-019:
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ECPAmps
GalvanicAmps
0
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...
Senes
98
June 4, 2004 - second run, no power
GalvanicVolts
ECPVolts
-0.168
-0.17
-0.172
-0.174
-0.176
-0.178
- I
I
I
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nu.w0
nn7
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0.006
0.005
0.004
0.003
0.002
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I~~~~~~~~~~~~
+ Series1
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-0.18
-0.182
-0.184
-0.186
|-|Sedesi
0.001
0
1
2
3
4
5
6
7
8
9
10
GalvanicAmps
ECP Amps
-0.0000114
n~
-0.0000116
: ,,;,
7
-,:,
,
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-0.0000118
-0.00005
-0.0000122
--- Series
-0.0001
i-- - Series1
-0.0000124-0 0000126
-0.0000128
-0.000013
-0.00015
-N NNVN
:
June 4, 2004 -third run, no power
Galvanic Volts
0.007
0.006
0.005
0.004
0.003
0.002
;- S~~~~~~~~~·
j_~~~~~~~
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t._.........
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0.001
0
V·Lcl
1
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2
3
4
5
6
--
7
8
9
10
-----------------------------
ECP Amps
Galvanic Amps
0
0 -
-0.000002
-0.00005
I1
2
3
4
5
6
7
s
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-0.000004
-0.0001
--
-.000006-
Seiesi
-0.000008
-0.00015
-0.00001
-0.0002
-0.000012
L_
99
Series
June 4, 2004 - fourth run, no power
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7
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0
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ECPVolts
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0
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112
Appendix D - X750-Pt Couple Graphs
May 27, 2004 - first run, no power
GalvanicVolts
ECP Volts
-0.05
0.006
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3
5
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11
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r----
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0
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114
May 28, 2004 - third run, no power
ECPVolts
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0.007
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115
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June 3, 2004 run, no power
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4
5
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7
8
9
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June 4, 2004 - first run, no power
ECPVolts
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June 4, 2004 - second run, no power
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0
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8
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June 4, 2004 -third run, no power
GalvanicVolts
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0.005
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1
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15
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June 4, 2004 - 1 MW run
GalvanicVolts
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0.006
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1
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2
3
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5
6
7
8
9
10
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-0.00005
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4
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June 4, 2004 - 2 MW run
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June 4, 2004 - 3 MW run
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June 4, 2004- 4 MW run
1
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June 7, 2004 run, no power
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June 8, 2004 - 4 MW run
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June 9, 2004 - 4 MW run
GalvanicVolts
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0
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June 10, 2004 - 4.35 MW run
ECPVolts
0
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June 11, 2004 - 4 MW run
ECPVolts
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June 14, 2004 - 4 MW run
ECPVolts
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June 15, 2004 - 4 MW run
GalvanicVolts
ECP Volts
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June 16, 2004 - 4 MW run
ECP Volts
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June
18, 2004 - 4 MW
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June 22, 2004 - 4 MW run
GalvanicVolts
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June 23, 2004 - 4 MW run
GalvanicVolts
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I
.'
'-.,
4 .
`7 I'
9 !0'
-0.00001
-0.0001
/1"
-
.-
Series 1
-0.000015
'
-0.00002
-0.00015
-0.000025
-0.00003
-0.0002
125
-0.000035
I..... ........
. ..
Fls i
-
'
......
lqs.
8SS
g E
....................
w<
Series1
June24, 2004 - 4 MW run
ECP Volts
GalvanicVolts
0
u.U4W
_
0.04
0.035
0.03
0.025
0.02
0.015
-0.01
-002
=
w
..
. _
, , , .117777777777777-
.
~,,z ~..,........
12
6*1~~~'
A 14 't -:rr
-P
F -e
i.
jlr
?.
0.01
-0.05
;-.:-'-I,
...
d-es-1
L:
&:
·
::
0.005
0
1
-r
1
2
3
4
ECPAmps
5
6
7
8
-·-,
9
10
Galvanic Amps
-0.000084
-0.000086
-0.000088
0.0004
0.00035
0.0003
0.00025
0.0002
0.00015
0.0001
0.00005
-0.00009
-,--- Sees1
-0.000092
-0.000094
-0.000096
-0.000098
-0.0001
I--- Series1
0
-0.00005
-0.0001
June 28, 2004 - 4 MW run
-0.03
:ECP Volts
-- L.0
-0.02
-0.021- .
GalvanicVolts
In
'-;]
,
W-
4-4.
.
-0.04
-005
-0.06
Z--
-0.07
L
-0.08
-n n
:
,
--
Seriesi
ns
0.04
0.035
0.03
0.025
0.02
0.015
0.01
0.005
0
-.-
....
1
ECPAps
0
2
3
4
5
6
7
8
9
Seriesi
10
GalvanicAmps
U
$,-~~~~~~At
-000005
-0.0001-Sees
-0.00005
-0.0001
-0.00015
-0.00015
-0.0002
-0.0002
|-
Series1
1
126
June 29, 2004 - 4 MW run
ECP Volts
GalvanicVolts
u.uzO
0.02
0.015
-4
.-
-
-Senesl
L
h.
-7
--.-- Series1
0.01
0.005
0
-8
1
2
3
4
ECPAmps
1
.
3
7
9
5
6
7
8
9
10
Galvanic Arnps
0
1 131 5
-0.00005
-0.00005
-0.0001
--
Sees
-0.00015
.....
.
Se es
.......
-0.00015
-0.0002
-0.0002
June 30, 2004 - 4 MW run
ECPVolts
0
-0.01-
GalvanicVolts
0.045
,
1
3 5
7
-0.02
8 11 13 15 17·
0.04·
-0.0~' :I_e__-Seriesli
'
'
-0.03-
0.035
0.03
0.025
..
0.02
0.015
-0.05
1
2
ECPAmps
-0.0000425
-0.000043
127
'
''-
,
Seriesl
0.01 _ _ _ _ _ _ _ _ _ _ _ _ _ _ _
0.005
-0.04
-0.000038
-0.0000385 1
-0.000039
-0.0000395
-0.00004
-0.0000405
-0.000041
-0.0000415 /
.
.-
3
4
5
6
5
11
8
Galvanic Amnps
0
3
7
5 1T
4
-0.0002
Series
...--11
-0.0004
-0.0006
-0.0008
-0.001
-0.0012
-0.0014
-0.0016
-0.0018
. 2
4a
" a
9
10
July 2, 2004- 4 MW run
ECPVolts
GalvanicVolts
0
0.07
0.06
I
-0.005
I
-0.01
v~
-0.02
v
^
-0.025
_
Sa | f;
0.04
_
+Senes1
| _Seriesl1
4,
,,,-,,.:, ;,;:
0.03
0.02
---.-
t
S
-0.03
0.01
-0.035
2
1
4
3
ECPAmps
5
6
7
9
8
10
GalvanicAmps
0
0
-0.00001
-0.00001
-0.00002
-0.00002
.- e Series1
-0.00003
|--
-0.00004
-0.00003
-0.00005
-0.00004
-0.00006
Series1
-0.00005
I
-
July 6, 2004 - 4 MW run
GalvanicVolts
ECPVolts
0.06-
0
0:05
-0005
-0.01
0.03 -
A
+u-~',
;s
:4.01:
-
+Senes
,~;0.0
0.02
-0.02
-0.025
*4
jV
e
I
0.03~
^
-- -*
I-
LiM fV
IZ
0.01
I'll
(
-
is
~1IM- 2
. "
3
4
U
0
-0.00001
-0.00002
-0.00003
-
-0.00005
-0.0000::,A
; ::,:A;~7 : :%?~4~~:- :
-.00008
-.00009
7
9
8
10
i
--
· --1 i--1--
--
rf-i
7T-
-0.00001
-000002
-0.00007
6
GalvanicAmps
ECP Amps
-0.00003
-0.00004
5
U
.A
-~.~
-Seesl
-0.00004
-0.00005
|'16'
j^
t
5
7'','s^d=z
'
1 T~~~~~~~~~~~t~.
-e Sediesl
-0.00006
-0.00007
-0.00008
-------
128
July 7, 2004 - 4 MW run
GalvanicVolts
ECP Volts
0.06
0
0.05
-0.005
-0.01
~~~....
-0.015
t
'
M
...
',
,
.
0.04
:
'
'
'
.:.'
: '
,,
.... ..
,,,,
-|- Series1
-0.02
0.03
---
Series1|
0.02
-0.025
0.01
-0.03
0
1
-0.035
2
3
4
5
6
7
8
9
10
Galvanic Amps
ECP Amps
0
-0.00005
-0.000052
-0.000054
-0.000056
-0.000058
-0.00006
-0.000062
-0.000064
-0.000066
-0.000068
3 . _
5
2 :3
3
1
_
*
4
1
Ž1
-0.00003
-Senes1
3
-000004
..
,
r
.
:
-0.00005
-0.00006
July 9, 2004 - 4 MW run
GalvanicVolts
ECP Volts
-0.
-0.005
.
.
1
o.
0.07 0.06 -
7
0.05
0.04
-0.01
-0.015
.
.. .
0.03
-0.02---Sees
0.02 -
-0.025
0.01
-0.03
0
1
-0.035
2
3
4
-0.0000504
-0.0000506 1
-0.0000508
-0.000051
-0.0000512
1.29
'3
.' -
:~7 i a "
;
... ..
. ;
'
,'ll, '
t . .4
Er-
r
I
e!f
'.
*_iZ-
6
7
8
9
10
8
0
i01
0
,, I -t9
. .,
5
GalvanicAmps
ECP Amps
-0.0000514
-0.0000516
-0.0000518
-0.000052
+ Senes
-Seeslj1
,...... ..
,
'
I
1
2 -S 4
5
6
7
-0.00001 -
I'
-0.00002
,,
--
Se-nesi
-0.00003
-0 00004
-0.00005
ioo o
-
~,i
o~'
i |-
Seiesl
July 12, 2004 - 4 MW run
ECPVolts
n
--
GalvanicVolts
0.06
-
0.05
-0.005
I- ,
;--
:n
r
-··-·
,pi
·
I
M W.]
-
0.04 .
Seriesi
0.03 -
002
001
-0.015
Li:}
0;x I"~·t"
-.02
1
-A'
-e-Series1
s
2
3
4
5
6
7
8
9
10
------------------------
·
July 15, 2004 -4 MW run
ECPVolts
GalvanicVolts
0
.044 4v'
0.06
4
,
0.05
-0.002
74
-0.004
"
' "
- Sees
U.U02
.
UA
v.jt kt7n.rtnt
vi
2 2_
.
-0.006
|Ss
-0008
-0.01
1
ECPAmps
0
-0.00001
-0.00002
-0.00003
-0.00004
-0.00005
-0.00006
-0.00007
-0.00008
AR
't
K-
` -" , :
f',
3
4
5
6
7
8
9
O
10
GalvanicAmps
0
. .. . . . "I
""', , "' -,-
-
2
-9-
"'
-0.0000
_
-.- Seriesi
-0.00006-
-0.00007-0.00006
130
Appendix E - ECP Data
Pt-Pt Couple
Power (W)
|
Temperature (°C)
ECP Volts (V)
ECP Amps (A)
Resistivity (f/cm)
Conductivity (S-cm)
0
300
-0.01498
-5.48E-06
2.73E+03
2.01E-09
0
300
-0.01426
-5.67E-06
2.52E+03
2.25E-09
0
300
-0.04651
-6.16E-05
7.55E+02
8.17E-08
0
300
-0.04386
-0.000050161
8.74E+02
5.74E-08
0
300
-0.0124
-1.53E-05
8.11E+02
1.89E-08
0
300
-0.01301
-1.88E-05
6.91E+02
2.73E-08
0
300
-0.0033
-2.38E-05
1.39E+02
1.71E-07
60
265.556
-0.00733
-1.16E-05
6.29E+02
1.85E-08
60
262.778
-0.0072
-1.16E-05
6.19E+02
1.88E-08
60
271.111
-0.00745
-1.28E-05
5.84E+02
2.18E-08
60
271.111
-0.00736
-1.27E-05
5.78E+02
2.20E-08
3.24E-08
1000000
270
-0.01687
-2.33943E-05
7.21E+02
2000000
271.111
-0.0169
-2.41E-05
7.01E+02
3.44E-08
3000000
268.333
-0.0165
-2.43E-05
6.80E+02
3.57E-08
4000000
265.556
-0.01608
-2.39267E-05
6.72E+02
3.56E-08
30000
223.889
-0.0076
-1.04964E-05
7.24E+02
1.45E-08
4000000
221.111
-0.0311
-2.28E-05
1.36E+03
1.67E-08
4000000
221.111
-0.021
-1.62669E-05
1.29E+03
1.26E-08
4350000
221.111
-0.0273
-2.24E-05
1.22E+03
1.84E-08
4000000
220.556
-0.00765
-1.95641E-05
3.91E+02
5.OOE-08
4000000
78.889
-0.07961
-2.55034E-06
3.12E+04
8.17E- 11
4200000
78.889
-0.1011
-3.20E-06
3.16E+04
1.01E-10
4200000
77.222
-0.094
-2.86E-06
3.28E+04
8.72E- 1
4200000
76.111
-0.0847
-3.08004E-06
2.75E+04
1.12E-10
4100000
248.889
-0.06409
-0.00282352
2.27E+01
1.24E-04
4000000
243.889
0.0948
4.53E-05
2.09E+03
2.16E-08
4000000
248.889
-0.0816
-4.02E-05
2.03E+03
1.98E-08
4000000
248.889
-0.06232
-4.72276E-05
1.32E+03
3.58E-08
4000000
248.889
4.29238
-4.90121E-05
8.76E+04
5.60E-10
4200000
248.889
-0.02601
-5.30289E-05
4.90E+02
1.08E-07
4000000
248.889
-0.0191
-0.000062117
3.07E+02
2.02E-07
4000000
248.889
-0.0229
-5.64E-05
4.06E+02
1.39E-07
-0.0172
-0.000066141
2.60E+02
2.54E-07
4000000
248.889
4300000
248.333
0.0151
-6.71 E-05
2.25E+02
2.98E-07
4300000
248.889
-0.00788
-7.24488E-05
1.09E+02
6.66E-07
4300000
248.889
-0.00586
-7.55122E-05
7.76E+01
9.73E-07
131
Zircaloy-Pt Couple
Conductivity
(S-cm)
Water
Resistivity
(f/cm)
Zr-2
Resistivity
(f/cm)
5.01E+04
2.00E-05
2731.956413
4.73E+04
4.48E+04
2.23E-05
2516.002908
4.23E+04
Power
(W)
Temperature
(°C)
ECP Volts
(V)
ECP Amps (A)
Resistivity
(f/cm)
0
300
-0.299655
-5.98554E-06
0
300
-0.278868
-6.22213E-06
0
300
-0.0764618
-5.98121E-05
1.28E+03
7.82E-04
754.5290399
5.24E+02
0
300
-0.207006
-4.59451E-05
4.51E+03
2.22E-04
874.384482
3.63E+03
-0.517888
-1.62577E-05
3.19E+04
3.14E-05
810.8709015
3.10E+04
0
300
0
300
-0.494585
-1.88151E-05
2.63E+04
3.80E-05
690.7353332
2.56E+04
0
300
-0.000335344
-2.34669E-05
1.43E+01
7.00E-02
138.9064276
1.25E+02
60
265.556
-0.180272
-1.31499E-05
1.37E+04
7.29E-05
629.2385612
1.31E+04
60
262.778
-0.169355
-1.29969E-05
1.30E+04
7.67E-05
618.5407593
1.24E+04
60
271.111
-0.213451
-1.45668E-05
1.47E+04
6.82E-05
584.0343052
1.41E+04
-1.43306E-05
1.42E+04
7.04E-05
578.2344992
1.36E+04
271.111
-0.203464
1000000
270
-0.150256
-2.51411E-05
5.98E+03
1.67E-04
721.1158274
5.26E+03
2000000
271.111
-0.137629
-2.62189E-05
5.25E+03
1.91E-04
701.3175641
4.55E+03
3000000
268.333
-0.122581
-2.65479E-05
4.62E+03
2.17E-04
679.6752388
3.94E+03
4000000
265.556
-0.111465
-2.60624E-05
4.28E+03
2.34E-04
672.0525605
3.60E+03
30000
223.889
-0.110251
-1.16626E-05
9.45E+03
1.06E-04
724.0577722
8.73E+03
4000000
221.111
-0.0549524
-2.38017E-05
2.3 1E+03
4.33E-04
1364.651575
9.44E+02
60
4000000
221.111
-0.0802635
-1.94661E-05
4.12E+03
2.43E-04
1290.965089
2.83E+03
4350000
221.111
-0.0913475
-2.06964E-05
4.41E+03
2.27E-04
1217.842055
3.20E+03
4000000
220.556
-0.0996254
-1.88003E-05
5.30E+03
1.89E-04
391.0223317
4.91E+03
4000000
78.889
-0.0496222
-2.62984E-06
1.89E+04
5.30E-05
31215.44578
1.23E+04
4200000
78.889
-0.0667444
-3.28554E-06
2.01E+04
4.98E-05
31611.92686
1.15E+04
4200000
77.222
-0.0619686
-3.08412E-06
1.37E+04
7.30E-05
32825.01126
1.91E+04
4200000
76.111
-0.0459537
-3.35691E-06
1.37E+04
7.30E-05
27499.64286
1.38E+04
4100000
248.889
-0.0262854
-0.00251044
1.05E+01
9.55E-02
22.69861733
1.22E+01
4000000
243.889
-0.0582953
-3.65238E-05
1.60E+03
6.27E-04
2094.948919
4.99E+02
4000000
248.889
-0.0572194
-0.000047771
1.20E+03
8.35E-04
2032.236855
8.34E+02
4000000
248.889
-0.22051
-4.83276E-05
4.56E+03
2.19E-04
1319.567372
3.24E+03
4000000
248.889
-0.0221873
-4.99286E-05
4.44E+02
2.25E-03
-87577.96544
8.80E+04
3.51E-03
490.4872626
2.06E+02
4200000
248.889
-0.017738
-6.22858E-05
2.85E+02
4000000
248.889
-0.017738
-6.22858E-05
2.85E+02
3.51E-03
307.4842636
2.27E+01
4000000
248.889
-0.0212619
-5.63743E-05
3.77E+02
2.65E-03
406.139265
2.90E+01
-0.0201533
-6.70171E-05
3.01E+02
3.33E-03
260.0504982
4.07E+01
4000000
248.889
4300000
248.333
-0.0148352
-6.69196E-05
2.22E+02
4.51E-03
225.1399297
3.45E+00
4300000
248.889
-0.00792714
-7.35919E-05
1.08E+02
9.28E-03
108.7664668
1.05E+00
4300000
248.889
-0.00632854
-7.51463E-05
8.42E+01
1.19E-02
77.60335416
6.61E+00
132
Zircaloy-X750 Couple
Power
(W)
0
0
0
0
0
0
0
60
60
60
60
1000000
2000000
3000000
4000000
30000
4000000
4000000
4350000
4000000
4000000
4200000
4200000
4200000
4100000
4000000
4000000
4000000
4000000
4200000
4000000
4000000
4000000
4300000
4300000
Temp.
(°C)
300
300
300
300
300
300
300
265.556
262.778
271.111
271.111
270
271.111
268.333
265.556
223.889
221.111
221.111
221.111
220.556
78.889
78.889
77.222
76.111
248.889
243.889
248.889
248.889
248.889
248.889
248.889
248.889
248.889
248.333
248.889
ECP Volts
(V)
-0.32544
-0.310167
-0.406071
-0.443373
-0.526066
-0.521837
-0.13123
-0.18912
-0.178039
-0.232452
-0.218974
-0.187857
-0.183208
-0.16769
-0.15127
-0.123451
-0.116688
-0.146594
-0.143138
-0.13432
-0.0505826
-0.0472375
-0.0614511
-0.0473553
-0.0043727
-0.0055496
-0.0780184
0.581803
-0.0374805
-0.0294753
-0.0294753
-0.032964
-0.030301
-0.0282423
-0.0128056
ECP Amps (A)
-6.3907E-06
-5.8804E-06
-1.7581E-05
-1.9162E-05
-2.0635E-05
-2.1159E-05
-1.5573E-05
-2.0649E-05
-2.0502E-05
-2.0979E-05
-2.1201 E-05
-2.1851 E-05
-2.129E-05
-2.1E-05
-2.0412E-05
-1.3681 E-05
-8.8681 E-06
-1.0286E-05
-1.2243E-05
-9.7601 E-06
-2.2916E-06
-2.5353E-06
-2.7856E-06
-2.9369E-06
-0.00044198
-8.9744E-05
-2.67E-05
-2.9896E-05
-3.5276E-05
-5.0426E-05
-5.0426E-05
-4.5026E-05
-5.6851 E-05
-5.5173E-05
-6.6737E-05
Resistivity
(I/cm)
5.09E+04
5.27E+04
2.31E+04
2.31E+04
2.55E+04
2.47E+04
8.43E+03
9.16E+03
8.68E+03
1.11E+04
1.03E+04
8.60E+03
8.61E+03
7.99E+03
7.41E+03
9.02E+03
1.32E+04
1.43E+04
1.17E+04
1.38E+04
2.2 1E+04
1.86E+04
2.21E+04
1.61E+04
9.89E+00
6.18E+01
2.92E+03
-1.95E+04
1.06E+03
5.85E+02
5.85E+02
7.32E+02
5.33E+02
5.12E+02
1.92E+02
4300000
248.889
-0.0090447
-7.1479E-05
1.27E+02
133
Conductivity
(S-cm)
1.96E-05
1.90E-05
4.33E-05
4.32E-05
3.92E-05
4.05E-05
1.19E-04
1.09E-04
1.15E-04
9.02E-05
9.68E-05
1.16E-04
1.16E-04
1.25E-04
1.35E-04
1.11E-04
7.60E-05
7.02E-05
8.55E-05
7.27E-05
4.53E-05
5.37E-05
4.53E-05
6.20E-05
1.01E-01
1.62E-02
3.42E-04
-5.14E-05
9.41E-04
1.71E-03
1.71E-03
1.37E-03
1.88E-03
1.95E-03
5.21E-03
7.90E-03
Water
Resistivity
(l/cm)
2731.956413
2516.002908
754.5290399
874.384482
810.8709015
690.7353332
138.9064276
629.2385612
618.5407593
584.0343052
578.2344992
721.1158274
701.3175641
679.6752388
672.0525605
724.0577722
1364.651575
1290.965089
1217.842055
391.0223317
31215.44578
31611.92686
32825.01126
27499.64286
22.69861733
2094.948919
2032.236855
1319.567372
-87577.9654
490.4872626
307.4842636
406.139265
260.0504982
225.1399297
108.7664668
Zr-2
Resistivity
(fQ/cm)
4.73E+04
4.23E+04
5.24E+02
3.63E+03
3.10OE+04
2.56E+04
1.25E+02
1.31E+04
1.24E+04
1.41E+04
1.36E+04
5.26E+03
4.55E+03
3.94E+03
3.60E+03
8.73E+03
9.44E+02
2.83E+03
3.20E+03
4.91E+03
1.23E+04
1.15E+04
1.91E+04
1.38E+04
1.22E+01
4.99E+02
8.34E+02
3.24E+03
8.80E+04
2.06E+02
2.27E+01
2.90E+01
4.07E+01
3.45E+00
1.05E+00
1.86E+04
6.36E+03
1.62E+03
8.16E+03
4.55E+03
4.35E+03
3.57E+03
3.87E+03
2.62E+03
3.36E+03
3.37E+03
3.13E+03
4.30E+02
1.08E+04
1.01 E+04
7.28E+03
8.46E+03
2.15E+04
2.45E+04
2.99E+04
2.52E+04
2.50E+01
2.53E+03
5.53E+01
2.40E+04
6.18E+02
1.12E+02
2.54E+02
2.97E+02
2.32E+02
2.83E+02
8.21 E+01
77.60335416
6.61E+00
4.23E+01
X-750
Resistivity
(f/cm)
8.61 E+02
7.93E+03
2.18E+04
AppendixF- Galvanic Data
Zircaloy-Pt Couple
Power (W)
0
0
0
0
0
0
0
60
60
60
60
1000000
2000000
3000000
4000000
30000
4000000
4000000
4350000
4000000
4000000
4200000
4200000
4200000
4100000
4000000
4000000
4000000
4000000
4200000
4000000
4000000
4000000
4300000
4300000
4300000
Temperature
(°C
300
300
300
300
300
300
300
265.556
262.778
271.111
271.111
270
271.111
268.333
265.556
223.889
221.111
221.111
221.111
220.556
78.889
78.889
77.222
76.111
248.889
243.889
248.889
248.889
248.889
248.889
248.889
248.889
248.889
248.333
248.889
248.889
Volts
)
0.000432307
0.000453008
0.000306517
0.000571941
0.000455308
0.000455078
0.000321928
0.000626835
0.000653976
0.000550628
0.000456173
0.000845032
0.00129392
0.00122568
0.00101661
0.00120437
0.000413545
0.000345235
0.000194122
0.000385255
0.000029057
2.93637E-05
2.71403E-05
0.000023997
0.00470505
0.00435627
0.00654239
0.00240877
0.00610354
0.00588922
0.00588922
0.0064987
0.00548663
0.00530971
0.00519534
0.00661039
Amps (A)
8.45972E-06
5.89889E-06
-2.9958E-05
-1.2436E-05
4.17026E-05
3.69525E-05
-2.0945E-05
3.20347E-06
2.21947E-06
4.61193E-06
4.22103E-06
-1.3343E-05
-1.4019E-05
-1.4504E-05
-1.5328E-05
-8.7315E-06
-2.5748E-05
-1.9471 E-05
-2.1699E-05
-1.9137E-05
-2.6274E-06
-3.1825E-06
-3.1931 E-06
-3.1524E-06
-0.00212674
-0.00019362
-4.7894E-05
-4.7134E-05
-4.6709E-05
-5.7866E-05
-5.7866E-05
-5.2489E-05
-5.6247E-05
-5.8961 E-05
-6.6223E-05
-6.7212E-05
Zircaloy-X750 Couple
Power (W)
0
0
0
0
0
0
0
60
60
60
60
1000000
2000000
3000000
4000000
30000
4000000
4000000
4350000
4000000
4000000
4200000
4200000
4200000
4100000
4000000
4000000
4000000
4000000
4200000
4000000
4000000
4000000
4300000
4300000
4300000
1:35
Temperature
(°C)
300
300
300
300
300
300
300
265.556
262.778
271.111
271.111
270
271.111
268.333
265.556
223.889
221.111
221.111
221.111
220.556
78.889
78.889
77.222
76.111
248.889
243.889
248.889
248.889
248.889
248.889
248.889
248.889
248.889
248.333
248.889
248.889
Volts (V)
0.000436447
0.000447181
0.000452318
0.000451551
0.000457224
0.000460215
0.00025101
0.000386712
0.000655586
0.000639256
0.0004942
0.000693536
0.000677359
0.000407106
0.000467673
0.00166905
-0.110251
0.00146351
0.00324626
0.00274225
0.00127099
3.28905E-05
0.000024687
0.000027907
0.00566463
0.0052296
0.00438808
0.00239865
0.00436593
0.00552334
0.00552334
0.00623294
0.00516812
0.00529675
0.00580743
0.00421093
I
Amps (A)
3.33718E-06
2.35226E-06
2.13312E-05
1.74476E-05
1.61925E-05
1.65482E-05
-6.84903E-06
-1.24261 E-05
-1.27474E-05
-9.64865E-06
-1.07538E-05
-8.76502E-06
-7.69927E-06
-8.2148E-06
-9.02906E-06
-1.00024E-05
-1.16626E-05
-6.42842E-06
-5.60431 E-06
-9.31305E-06
-4.20061 E-06
-2.86337E-06
-2.77583E-06
-2.91526E-06
-0.000114533
-0.000085416
-0.000194056
-4.53562E-05
-0.000200685
-4.53559E-05
-4.53559E-05
-4.13855E-05
-4.73973E-05
-4.69493E-05
-5.95676E-05
-5.07742E-05
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