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Nuclear Engineering and Design 115 (1989) 207-218

North-Holland, Amsterdam

207

EFFECT OF DECONTAMINATION ON AGING PROCESSES AND CONSIDERATIONS


FOR LIFE EXTENSION *
D.R. D I E R C K S
Materials and Components Technology Division, Argonne National Laboratory, Argonne, IL 60439, USA
Received 1 March 1988

The basis for a recently initiated program on the chemical decontamination of nuclear reactor components and the possible
impact of decontamination on extended-life service is described. The incentives for extending life beyond the present 40-year
limit are discussed, and the possible aging degradation processes that may be accentuated in extended-life service are
summarized. Chemical decontamination processes for nuclear plant primary systems are reviewed with respect to their
corrosive effects on structural alloys, particularly those in the aged condition. Available experience with chemical cleaning
processes for the secondary side of pressurized water reactor (PWR) steam generators is also considered. Overall, no severe
materials corrosion problems have been found that would preclude the use of these chemical processes, but concerns are raised
with respect to corrosion-related problems that may develop during extended service.

1. Introduction

This paper describes the basis for a recently initiated


program on the decontamination of nuclear reactor
components and the possible impact of decontamination on extended-life service. The use of chemical decontamination processes in nuclear power plants to
reduce worker exposures during repairs and maintenance continues to increase. At the same time, there is
growing interest in extending the life of existing nuclear
plants, beyond their present 40-year licensing period.
Concerns about the possible adverse effects of repeated
decontaminations on the remaining service life of aged
components must be addressed before operating licenses
for extended life can be renewed. Although a wide
variety of nuclear power plant components are subject
to aging effects of one kind or another, the present
paper is specifically concerned with metallurgical and
chemical effects in components that are likely to be
exposed to decontamination solutions, i.e. selected pressure boundary components and reactor internals. Chemical cleaning of steam generators to remove sludge and
reduce denting, though not strictly a decontamination
process, is also included.
* Work supported by the U.S. Nuclear Regulatory Commission, Office of Nuclear Regulatory Research, under contract
W-31-109-Eng-38.

2. Plant life extension and component aging


The duration of a license for a nuclear power plant
in the United States was set at a maximum of 40 years
by the Atomic Energy Act of 1954, with possible renewal at the end of that time period [1]. Several studies
[2-4] have found that service life extensions beyond this
40-year limit are technically feasible and that the economic incentives are considerable. A 1982 evaluation
performed for the Electric Power Research Institute
(EPRI) concluded that such life extension could be
cost-effective even at a plant refurbishment cost of $30
million to $1 billion [3]. It has also been noted that
present 40-year operating licenses for nuclear power
plants in the U.S. will begin to expire in the year 2000,
and by 2010 the expiration dates for approximately 75
reactors will be within the 12-year planning horizon for
replacement generating capacity [5]. It is therefore not
surprising that the U.S. Nuclear Regulatory Commission (USNRC) has already begun to seriously examine
the safety implications associated with nuclear power
plant life extension [6].
The major concern with respect to the possible
licensing of nuclear plants for operation beyond 40
years is that of component aging. In terms of metallurgical effects, such aging can take several forms, including low-temperature sensitization of stainless steels,
long-term embrittlement of cast duplex stainless steels,
environmental fatigue damage to carbon steel piping

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D.R. Diercks / Effect of decontamination on aging processes

materials, and radiation-induced embrittlement and intergranular stress-corrosion cracking (IGSCC) of reactor internal components.
It has been recognized only relatively recently that
sensitization of stainless steels can occur after prolonged exposures (of the order of years) to temperatures
of 400C or less [7,8]. This process, known as low-temperature sensitization, generally requires an initial brief
exposure to higher temperatures (600-800C) to
nucleate the carbide particles that subsequently grow at
lower temperatures. Just as with conventional sensitization, this precipitation process depletes the grainboundary regions of Cr and leaves them more susceptible to intergranular corrosion. Low-temperature sensitization is of concern in nuclear plant coolant piping and
reactor internals operating at temperatures of
250-288C, particularly under conditions of extendedlife operation.
Another aging phenomenon, sometimes known as
475C embrittlement, can occur in ferritic and cast
duplex stainless steels. When these steels are exposed
for extended periods of time to temperatures in the
range from 300 to 500C, the Cr-rich a' phase precipitates within the ferrite, resulting in severe embrittlement. It now appears that a similar series of time-dependent precipitation phenomena may occur at light
water reactor (LWR) operating temperatures in the
ferrite phase of cast duplex stainless steels such as CF-3
and CF-8, which are used to fabricate nuclear plant
primary coolant piping as well as valve and pump
casings [9]. Again, this very slow aging process is of
greatest concern under conditions of extended-life operation.
Carbon steel piping materials, particularly in boihng
water reactors (BWRs), are subject to time-dependent
low-cycle fatigue damage caused primarily by thermal
cycling. The American Society of Mechanical Engineers
(ASME) Boiler and Pressure Vessel Code Section III
includes fatigue design curves to deal with this problem,
but these curves do not allow for the deleterious effects
of the operating environment [10]. Experimental studies
have suggested that the safety factors built into the
ASME Code design curves may be inadequate for
structural carbon and low-alloy steels in a BWR environment [11,12]. Since this environmental fatigue
damage accumulates with length of service, it is included here as an aging phenomenon. Recent work
indicates that the problem may be related to the sulfur
content of steel [13].
The embrittlement of reactor pressure vessels and
internal components due to neutron irradiation may
also be considered to be an aging phenomenon of sorts.

This embrittlement process is generally characterized in


terms of an increase in the transition temperature between brittle behavior observed at lower temperatures
and ductile fracture at higher temperatures. This transition temperature increases with increasing neutron
fluence (and therefore service time), and it has also been
found to be strongly influenced by the presence of
certain impurities such as Cu and Ni in the steel.
Control of these residual element levels has greatly
reduced in the embrittlement problem in the newer
reactor pressure vessels, but older vessels will require
careful monitoring, particularly if extended-life operations are attempted.
A related time-dependent failure process that primarily affects BWR core components is that of irradiation-assisted IGSCC. This failure mode can occur in
high-temperature water containing short-lived oxidizing
species such as H 2 0 2 and the simultaneous presence of
a gamma and neutron irradiation field. It appears to
associated with the grain-boundary segregation of
impurity elements such as sulfur, silicon, and phosphorus, but it does not require a sensitized microstructure. Components subject to this failure model include
type 304 SS neutron source holders, control rod absorber
tubes, and in-core instrument tubes [14]. No data are
available on the effects of decontamination on the
sucseptibility of in-core components to irradiation-induced IGSCC.

3. Chemical decontamination
3.1. General background
3.1.1. Nature of contaminant oxides
The radioactive contamination presents on the
surfaces of nuclear reactor cooling circuit components
consists of a complex mixed oxide made up primarily of
transition-metal spinels. The principal radionuclides
present in this film include 58C0, 6C0, SlCr, 55Fe, 59Fe,
54Mn, 63Ni, and 65Zn. Of these, 6C0 is the most
important, since it accounts for approximately 80% of
the exposure received by U.S. nuclear plant workers
during operation, inspection, and maintenance activities
[151.
The radioactive oxides can divided into two types,
"deposited" and "grown-on" [16]. The deposited oxides
are produced when non-radioactive surface oxides
formed on components upstream from the core are
released into the circulating coolant by corrosion or
erosion processes as suspended particles or dissolved
ions. Some of these particles or ions deposit or precipi-

D.R. Diercks / Effect of decontamination on aging processes

tate in the core, become activated, and are again released


into the coolant. They then redeposit on the surface of
downstream reactor components to produce radioactive
contamination. Once these oxides have redeposited, they
can pick up additional activity by ion-exchanging dissolved radioactive species from the coolant. The components most commonly contaminated in this way are the
recirculation piping and pumps in BWRs and the hot-leg
primary piping and steam generator channel heads in
pressurized water reactors (PWRs).
The grown-on oxides result from the in-situ corrosion of cooling circuit surfaces. These oxides remain on
the component surfaces where they form and are never
exposed to radiation in the core. Instead, they become
radioactive by absorbing active species from solution
and incorporating these radionuclides into their structure as they grow.
The deposited oxide normally overlays the grown-on
oxide, but the layers are seldom distinct. In BWRs, the
major source of corrosion product input is from the
coolant feed train (feedwater heaters and drains), and a
relatively thick contaminated layer made up primarily
of deposited Fe and Ni oxides is formed. In PWRs, on
the other hand, all of the corrosion products arise
within the primary circuit, which is made up of corrosion-resistant materials such as type 304 stainless steel
and Inconel 600. The contaminant oxide therefore consists primarily of grown-on oxide and is typically much
thinner (approximately one-tenth of the BWR oxide
thickness). This oxide also contains a substantially
greater percentage of Cr and is generally more difficult
to dissolve during chemical decontamination.
The oxidation state of the Fe contained in the oxide
layer is an additional consideration in decontamination,
particularly for BWRs. In the relatively oxidizing water
chemistry of BWRs, an outermost layer consisting
largely of Fe in the + 3 valence state as Fe203 and
FeOOH is commonly present. With increasing depth
into the oxide layer, the Fe gradually transforms to the
mixed + 2 and + 3 states (Fe304), and finally to the + 2
state (FeCr204) in the thin grown-on oxide layer adjacent to the reducing conditions of the underlying base
metal. This innermost grown-on layer typically contains
relatively little 60Co, Since this oxide formed during the
early stages of corrosion before significant quantities of
this radionuclide had been generated. However, 6Co
tends to concentrate in the intermediate Fe304 layer.
This occurs because 60Co ions exist in the + 2 oxidation
state in a BWR water chemistry, and the Fe +2 in Fe304
is more conducive to the incorporation of these ions
than the Fe +3 in the Fe203 outer layer. Consequently,
effective decontamination of BWR components requires

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removal of both the outer and intermediate deposited


oxide layer.
3.2.2. Decontamination experience in the U.S.

The radiation field produced by the contaminant


oxides described above is of principal concern during
reactor outages for maintenance or repair, since it limits
the working time of personnel in the region. In fact,
radiation exposure represents a specific cost, quoted to
be as much as $5000 to $7000 per man-rem [16,17], that
electrical .utilities must bear during maintenance and
repair procedures. Decontamination of primary loop
components to reduce radiation fields and lower the
man-rem exposure is therefore of vital economic interest
to utilities. For example, based upon experiences with
the Dresden 3 and Quad Cities 1 and 2 reactors, Commonwealth Edison Company reports average net savings of $1.25 million from decontamination of recirculation piping preparatory to performing in-service inspection and repair work [19,20]. Reduction of the radiation
exposure of nuclear plant personnel through effective
decontamination is also consistent with the NRC objective of maintaining such exposure as low as reasonably
achievable (ALARA).
Experience in the United States with the chemical
decontamination of commercial nuclear power reactors
is summarized in table 1. This tabulation is not intended to be exhaustive, but it does include a large
majority of the chemical decontaminations that were
performed through the end of 1986. Most of the decontaminations were carried out on BWR primary
coolant recirculation systems (PCRS) and reactor water
clean-up systems (RWCU). In PWRs, the components
most commonly decontaminated have been steam generator channel heads. Almost all of these decontaminations were carried out immediately prior to maintenance
or repair work to reduce worker exposure. The principal
decontamination processes were CAN-DECON, NS-1,
and, in more recent years, LOMI. It is apparent from
the table that chemical decontamination is becoming an
increasingly common practice.
During a nuclear reactor decontamination, the chemical solutions are likely to come into contact with a
number of different structural alloys. The more widely
used of these alloys are listed in table 2 along with
examples of components in which they are utilized.
Although core decontaminations with the fuel in place
are not yet being routinely performed in the United
States, they have been performed in Canada (Douglas
Point and Pickering Candu Reactors) and the U.K.
(Winfrith reactor), and are of growing interest in the
U.S. Commonwealth Edison has estimated that as much

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D.R. Diercks / Effect of decontamination on aging processes

Table 1
Summary of experience with chemical decontamination of commercial nuclear power reactors in the United States
Date

Plant

Process

Components
decontaminated a

6/76
4/77
9/77
10/79
5/80
3/81
4/81
10/81
12/81
4/82
4/82
5-8/82
12/82
4/83
3-4/83
10/83
10/83
1/84
3/84
4/84
4/84
5/84
7/84
7-8/84
9/84
11/84
12/84
1984
10/85
11/85
5/86
6/86
7/86
11/86
12/86

Dresden 1
Peach Bottom 3
Peach Bottom 2
Vermont Yankee
Brunswick 2
Nine Mile Point
Brunswick I
Vermont Yankee
Brunswick 1
Peach Bottom 2
Nine Mile Point
Nine Mile Point
Hatch 1
Peach Bottom 3
Vermont Yankee
Quad Cities 2
Dresden 3
Pilgrim
Monticello
Quad Cities I
Brunswick 2
Millstone 1
Peach Bottom 2
Pilgrim
Dresden I
Dresden 2
Cooper
Quad Cities 2
Vermont Yankee
Dresden 3
Quad Cities I
Oyster Creek
Brown's Ferry 1,2,&3
Quad Cities 2
Dresden 2

NS-1 (conc.)
NS-1 (conc.)
NS-1 (cone.)
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
CAN-DECON
NS-1 (dilute)
LOMI
CAN-DECON
Citrox
CAN-DECON
CAN-DECON
NS-1 (dilute)
NS-1 (cone.)
NS-1 (dilute)
Citrox (dilute)
CAN-DECON
LOMI
LOMI
CAN-DECON/LOMI
LOMI
7 processes compared
LOMI
LOMI

1964
1976
9/82
11/82
4/83
8/83
8/84
5/85
1985
1/86
6-8/86
1986

Shippingport
Surry
Surry 2
Surry 2
Girma
Millstone 2
Palisades
Millstone 2
Indian Point 3
Connecticut Yankee
H.B. Robinson
Millstone 2

Turco 4502/4521
NS-1 (conc.)
CAN-DECON
LOMI
CAN-DECON
OZOX
CAN-DECON
Citrox A
LOMI
CAN-DECON
LOMI
OZOX-A

Years since
startup

Boiling water reactors

Primary system test loop


RWCS
RWCS
RWCS
RWCS
5 primary recirc, pumps
RWCS
RWCS
aux. steam system
RWCS
2 primary recirc, pumps
PCRS
RWCS
RWCS
PCRS
PCRS
PCRS and RWCS
PCRS
PCRS and RWCS
RWCS
RWCS
PCRS and RWCS
PCRS
PCRS and RWCS
PCRS
PCRS
PCRS
RWCS
PCRS and RWCS
PCRS and RWCS
2 irradiated fuel assemblies
PCRS
6 RWCS pumps
PCRS and RWCS
PCRS and RWCS (hot leg)

16
3
3
7
4
4
4
9
5
8
12
12
7
8
10
11
12
11
13
12
8
14
10
12
24
14
10
12
13
14
14
17
9-12
14
16

Pressurized water reactors

PCRS
Evaporator
Channel head (cold leg)
Channel head (hot leg)
Channel heads
Channel heads
Channel heads
Channel heads
Channel heads
Channel heads
Isolated primary pump
Channel heads

a PCRS-primary coolant recirculation system. RWCS = reactor water cleanup system.

7
3
9
9
13
8
13
10
9
18
15
11

D.R. Diercks / Effect of decontamination on aging processes


Table 2
Examples of nuclear reactor structural alloys likely to be
exposed to chemical decontamination or cleaning solutions
Alloy
Austenitic stainless steels
Types 304 and 304L
Types 316, 316L, and 316NG
Types 308, 308L, and 309

Cast duplex stainless steels


CF-3; CF-8; CF-8M

Application
Primary coolant piping
Primary coolant piping
Corrosion-resistant
cladding on pressure
vessels and piping
Primary coolant piping;
valve and pump casings

Carbon steels
A285; A515, Grade 60; A570

Steam generator support


plates
A106, Grade B; A333, Grade 6 BWR piping
Steam generator shells
A516
A516, Grade 70 (308L SS clad) PWR piping
Low-alloy steels
Steam generator shells
A302, Grade B;A533, Type A
Steam generator tube
A508
sheets
Reactor pressure vessel
A508, Class 2
forgings
Reactor pressure vessel
A533, Type B
plate
Nickel-base alloys
PWR steam generator
Inconel 600
tubing;
primary coolant piping
Core structural
Inconels 625,718, and X
components
Core structural
Inconel X-750
components;
BWR jet pump beams
Corrosion-resistant
Inconels 82 and 182
cladding on pressure
vessel nozzles
Special purpose alloys
Nuclear fuel cladding
Zircaloy-2 and -4
Control element drives
Haynes Stellite 6B
Weld-deposited hard
Haynes Stellite 6
facing on pumps
and valves

as 50% of the radioactive deposits entrained in the oxide


film of primary system piping has as its source the fuel
cladding. Thus, a full system decontamination including
fuel would substantially retard the subsequent build-up
of radiation levels [20]. For this reason, Zircaloy cladding material is included in table 2. The high-strength
Ni-base Inconel alloys 718 and 625, which are used for

211

structural applications, are included for the same reason.


It should be noted that several of the alloys listed in
table 2 are susceptible to the long-term metallurgical
aging effects previously described. For example, the
austenitic stainless steels (SS) and, to a lesser extent,
Incoloy 600, are subject to low-temperature sensitization, although type 316 N G SS has been specifically
developed to resist sensitization. Possible aging embrittlement of the case duplex stainless steels CF-8 and
CF-3 has .already been discussed, as has the low-cycle
environmental fatigue of the carbon steel piping materials and the neutron irradiation embrittlement of the
low-alloy pressure-vessel steels.

4. CAN-DECON process

4.1. Description of the CAN-DECON process


The CAN-DECON process, which was developed by
Atomic Energy of Canada Ltd. during the early 1970s
[21], has been the most widely used chemical decontamination process in the United States. The process
was successfully demonstrated in August 1975 when it
was used to decontaminate the entire primary system of
the Douglas Point Candu reactor, including the fuel.
The process was first used on a commercial basis in the
United States to decontaminate the reactor water cleanup system of the Vermont Yankee BWR in late 1979.
Since that time, more than 20 decontaminations of
BWRs and PWRs have been carried out in the United
States using CAN-DECON.
The principal active chemical reagent used in the
CAN-DECON process was originally Nutek L-106, sold
by Nuclear Technology Corp. of Amston, CN [22].
Since 1977, the reagent LND-101A, developed by LN
Technologies, has been utilized. This proprietary reagent consists of a mixture of reducing organic acids
(including oxalic acid) to dissolve the radioactive oxide
films present on the components and a chelant to
prevent redeposition of dissolved radioactive metal ions.
As discussed in the next section, LN Technologies has
recently introduced two alternative solutions to LND101A to avoid the possible intergranular attack of
stainless steels that has been observed under severe
laboratory conditions [21].
The CAN-DECON decontamination process is carried out by first adjusting the circulating reactor coolant
to proper chemistry (neutral pH, low conductivity, and
low dissolved oxygen) through ion exchange and chemical addition [23]. The solid LND-101A reagent is then

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D.R. Diercks / Effect of decontamination on aging processes

injected into the circulating coolant to achieve a concentration of approximately 0.1 wt%. The organic acids
attack and dissolve the contaminant oxide film, and the
metal ions released combine with the chelating agent.
Continuous on-line regeneration of the decontaminating
solution is accomplished by passing a side stream of
active solution through a filter and cation resin column
to remove particulate and dissolved ions. The decontamination treatment is typically performed at a
coolant temperature of 120C, although decontaminations have successfully been carried out at temperatures
from approximately 80 to 135 o C [24]. Decontamination
times normally range from 24 to 100 h [25].
The higher-Cr oxide films formed on contaminated
PWR components are not soluble in the LND-101A
reagent and its modifications, since the Cr is present in
these films as insoluble Cr 3+. An alkaline potassium
permanganate (AP) solution designated LND-104 has
therefore been developed to oxidize the Cr 3 ions to the
soluble Cr 6 state. In decontaminating a PWR, the
reducing LND-101A treatment described above is typically preceeded by or are alternated with one or more
oxidizing LND-104 treatments.
4.2. Corrosion studies on C A N - D E C O N

The CAN-DECON reagents and related dilute


organic acid decontamination solutions have been extensively tested to determine their possible corrosive
effects on nuclear reactor structural materials. Some of
the first tests were conducted on a 0.012 M oxalic
acid/0.005 M citric acid solution developed by General
Electric Company for the possible decontamination of
BWRs [26]. The general corrosion rates observed in
these tests were acceptable for all of the alloys tested,
with the greatest penetrations observed for low-alloy
steels. Grain-boundary etching and pitting were observed in welded and low-temperature sensitized type
304 SS specimens from one heat of material. In addition, one of three welded plus furnace-sensitized Inconel 600 specimens shows slight pitting in the case
metal, and two of three tempered Inconel X-750 specimens exhibited isolated intergranular attack (IGA).
Some indication of enhanced IGSCC was seen in sensitized type 304 SS specimens exposed to BWR conditions after decontamination, but the results were not
clear-cut.
Concerns about the possible detrimental effects of
the CAN-DECON LND-101A reagent in particular on
LWR structural alloys were raised in early 1982 in
conjunction with the decontamination of the Nine Mile
Point 1 BWR primary coolant recirculation system

(PCRS) [27]. A Task Force formed to study the Nine


Mile Point I safe-end cracking failures concluded that
" . . . the 1982 total recirculation system decontamination
does not appear to have exacerbated the observed
cracking" [28]. Its only clear effect, insofar as the cracking was concerned, was " . . . the increase in sensitivity
for inspection of cracks which already existed in the
system". However, some of the piping welds were heavily
electropolished after decontamination to further reduce
radiation levels, and this electropolishing treatment removed some of the original inner surface where IGA
induced by the decontamination process might have
occurred. Furthermore, the failed piping was removed
immediately after decontamination and therefore never
saw actual reactor service. The Task Force report cautioned that longer term exposures after decontamination might reveal effects related to subsequent crack
lmtlat~on.
Subsequent laboratory tests of the CAN-DECON
LND-101A reagent and its possible contribution to the
corrosion of sensitized type 304 SS, Inconel 600, and SA
533 Grade B pressure-vessel low-alloy steel were intiated by the General Electric Company [29]. Decontamination processing for 48 h at 120C in a 0.1
wt% solution of LND-101A produced relatively high
corrosion rates of about 0.18 m m / d a y in the low-alloy
steel, but the rates for the other two alloys were of the
order of 10 -3 mm/day. However, the decontamination
process was found to have produced IGA to a depth of
about 0.2 mm (2 to 3 grain diameters) in the type 304
SS specimens and 0.09 mm ( - 3 grain diameters) in the
Inconel 600 specimen. In addition, surface pitting was
observed in these latter two materials. It was noted that
the IGA might be mitigated by increasing the ferric ion
concentration in solution. Subsequent constant extension rate tensile (CERT) tests at 288C (550F) in
water containing 0.2 ppm dissolved oxygen indicated an
increased susceptibility to stress corrosion cracking
(SCC) in the sensitized type 304 SS. In the case of
field-decontaminated type 304 SS BWR pipe welds,
shallow intergranular attack (IGA) and pitting were
observed but the IGSCC resistance was not affected.
As a follow-up to the General Electric study, London
Nuclear conducted a comprehensive review of general,
galvanic, crevice, and pitting corrosion data and SCC
test results for the CAN-DECON process obtained by
themselves and others [24,30-33]. The alloys evaluated
included several carbon steels, austenitic and ferritic
stainless steels, nickel-base alloys, Zircaloy-2, and Stellite 6. This review, plus supplemental tests conducted by
London Nuclear and Ontario Hydro, concluded that
the LND-101A solution does not, in general, produce

D.R. Diercks / Effect of decontamination on aging processes


undesirable corrosion effects in the evaluated alloys. In
the sensitized conditions, type 304 SS and Inconel 600
showed a significant susceptibility to IGSCC after a
500-h treatment when the solution contained no ferric
ions. However, this problem was eliminated by the
addition of ferric ions at concentrations of - 50 to 80
ppm. The enhanced I G A and IGSCC susceptibility
previously observed in the General Electric studies was
attributed to a lack of ferric ions in solution, and
London Nuclear introduced a reformulated version of
LND-101A, known as Rem-E-D, which contains ferric
citrate additions to ensure a sufficiently high concentration of ferric ions during the initial stages of decontamination. In addition, London Nuclear introduced
a modified version of reagent LND-101A known as
LND-107, in which the oxalic acid implicated in I G A
under certain severe conditions, was removed [22].
Additional crack initiation and growth studies are
presently being conducted by General Electric Company to further evaluate the possible effects of CANDECON on post-decontamination IGSCC [34]. To date,
IGSCC failures have been reported in cyclic loading
tests on precracked 304 SS welded pipe specimens tested
under simulated BWR conditions after pre-exposure to
the CAN-DECON with ferric ion additions and
A P / C A N - D E C O N decontaminations. In both cases, it
was concluded that the CAN-DECON processes produced no obvious deleterious effects on failure times. In
contrast, simultaneous fracture-mechanics crack-growth
tests indicated statistically significant increases in crack
growth rate as a result of CAN-DECON plus ferric ion
treatments for Inconel 600, 182, and X-750 specimens,
all tested in the low-temperature sensitized condition. It
was concluded from these latter tests that, in contrast to
the previous findings of London Nuclear, the CAN-DECON treatment caused perceptible degradation in
IGSCC resistance for several alloys, even when a high
ferric ion concentration is maintained in the decontamination solution.
A related study of the corrosive effects of generic
dilute decontamination solutions containing oxalic acid,
citric acid, ferric citrate, and ethelenediaminetetraacetic
acid (EDTA) on sensitized type 304 SS has recently
been completed [35]. The study found that of the three
basic solution types considered, citric acid/oxalic acid
solutions were the most corrosive to sensitized type 304
SS, followed by citric acid/oxalic a c i d / E D T A solutions and citric a c i d / E D T A solutions. In all cases,
removing the oxalic acid from the solutions lowered
their corrosivity, In addition, pitting and I G A attack
occurred only in solutions containing oxalic acid. Although adding EDTA to citric acid/oxalic acid solu-

213

tions lowered their corrosivity, it also appeared to promote IGA. Adding 70-90 ppm ferric ion as ferric
citrate to the citric acid/oxalic a c i d / E D T A solutions
reduced I G A to insignificant levels. However, similar
ferric ion additions to citric acid/oxalic acid solutions
(no EDTA) can increase or decrease surface attack,
depending upon the initial concentration of oxalic acid
present. Citric a c i d / E D T A solutions caused negligible
damage with or without ferric ion additions. These
results thus support London Nuclear's contention that
I G A can be controlled by ferric ion additions to CANDECON LND-101A (i.e. the reformulated Rem-E-D)
or by removing the oxalic acid (LND-107). They do not
explain the enhanced IGSCC seen by General Electric
researchers in Inconels 600, 182, and X-750 exposed to
LND-101A with ferric ion additions.
Overall, the experimental corrosion data obtained on
the CAN-DECON process present a somewhat confused picture. The observed general corrosion rates appear to be acceptable for most alloys tested, although
corrosion inhibitor additions may be required to protect
carbon and low-alloy steels. Early work conducted by
General Electric clearly implicated CAN-DECON in
the I G A and IGSCC of sensitized type 304 SS, but later
London Nuclear and Ontario Hydro studies found that
these effects could be eliminated through ferric ion
additions. Recent results obtained by Chalk River on
generic solutions related to CAN-DECON LND-101A
support this finding, at least for sensitized type 304 SS.
However, additional experiments carried out by General Electric have found that the CAN-DECON treatment can accelerate crack growth in several alloys, even
with ferric ion additions. N o data are available on the
effects of CAN-DECON on alloys subjected to prior
long-term aging.

5. LOMI process

5.1. Description of the L O M I process


The LOMI (low oxidation-state metal ion) process
was developed by the U.K. Central Electricity Generating Board (CEGB) in the later 1970s. The process
utilizes V 2+ ions in the form of vanadium picolinate to
reduce Fe 3+ ions in the corrosion product scale to the
more soluble Fe 2+ state, with the V 2+ ions being
oxidized to V 3+. The LOMI decontamination process is
applied in a manner similar to that used for the CANDECON process [23]. However, reactor coolant temperatures are typically lower (80-90 C), and decontamination times are very short - typically of the order of 1-3

214

D.R. Diercks / Effect of decontamination on aging processes

h [25]. A prior preoxidizing alkaline permanganate (AP)


or nitric acid permanganate (NP) step is required to
remove the higher-Cr films present on PWR components. As with the CAN-DECON process, this preoxidation step oxidizes the insoluble Cr 3+ ions to the
soluble Cr 6 state, and they are dissolved in the subsequent LOMI treatment.
5.2. Corrosion studies on the L O M I process

During the development of the LOMI decontamination process, corrosion studies were conducted by the
CEGB-Berkeley Nuclear Laboratories [36]. Alloys included EN 2 carbon steel, several stainless steels, Inconels 600 and 800, Zircaloy 2, and several stainless steel/
carbon steel weldments. Corrosion rates were found to
be negligible for all but the carbon steel, the type 410
SS, and the weldments. The type 410 SS corroded at a
rate of 0.47-0.66 # m / h , and the rate for the weldments
was less than 0.005 # m / h . The carbon steel corroded
only when the reducing capacity of the reagent had
been exhausted, i.e. when all of the V 2 ions had
oxidized to V 3+. The observed average corrosion rates
for the carbon steel over the entire 3.2-h exposure were
0.31 to 0.72/~m/h.
Additional corrosion tests of the LOMI solution
were conducted by Pacific Northwest Laboratories
(PNL) under EPRI sponsorship [37]. Prefiimed type 304
SS specimens were exposed to simulated BWR (NP,
LOMI, and N P / L O M I ) and PWR (NP, LOMI, A P / N P ,
N P / L O M I , and A P / N P / L O M I ) decontamination
treatments. Prefilmed Inconel 600 specimens were exposed only to the simulated PWR treatments. The extent of general corrosion observed was very small in all
cases. The greatest observed thickness losses for both
alloys, of the order of 0.2 /~m, were produced by the
N P / L O M I and A P / N P / L O M I processes. No differences were observed between samples not rinsed and
stored wet for 14 days after decontamination and those
rinsed and stored dry.
U-bend and CERT tests were conducted on both
alloys in both the lightly and heavily sensitized conditions after various prefilming and LOMI, N P / L O M I ,
and A P / N P / L O M I treatments. No IGA or SCC was
seen under any of the test conditions. Scanning electron
microscope (SEM) examinations of non-decontaminated, decontaminated, and post-filmed type 304
SS specimens indicated that film removal and some
minor uniform corrosion occurred in the case of the
A P / N P / L O M I treatment. However, the surfaces appeared to repassivate during post-filming. Slight pitting
was observed on one of the Inconel 600 specimens after

the NP treatment, and more extensive pitting was seen


after the N P / L O M I treatments. In all cases, the pitting
repassivated and did not propagate during post-filming.
No IGA was observed in either of the alloys after any
of the filming or decontamination treatments.
Additional corrosion studies of the LOMI process
were conducted at General Electric in 1985 on furnacesensitized type 304 SS, low-temperature sensitized Inconel 600, and quenched and tempered SA533 Grade B
low-alloy steel specimens [29]. The general corrosion
produced by the LOMI decontamination was found to
be of the order of 0.1 /~m for the type 304 SS and
Inconel 600 specimens and 20 /~m for the low-alloy
steel. In all cases, these rates were an order of magnitude or more lower than the rates observed for CANDECON decontaminations of similar specimens. SEM
examinations of the surfaces of the LOMI-treated specimens revealed little change from the prefilmed condition for the type 304 SS and Inconel 600 specimens and
moderate uniform corrosion in the case of the SA533
Grade B specimens. No tendency toward accelerated
cracking or IGSCC was seen in CERT tests, with observed values of maximum stress, reduction in area,
total elongation, and time to failure being similar for
LOMI-decontaminated and control specimens.
A further corrosion study of the LOMI process was
conducted by General Electric simultaneously with their
investigation of the CAN-DECON process discussed
above [34]. As with the CAN-DECON treatment, no
deleterious effects of LOMI or A P / L O M I treatments
were seen on crack growth behavior in precracked
welded type 304 SS pipe specimens. In fact, failure
times for the LOMI and A P / L O M I treated specimen
were significantly longer than predicted. In fracture
mechanics crack-growth tests, LOMI-treated specimens
again generally exhibited crack growth rates similar to
or less than untreated control specimens. The exceptions were sensitized Inconel 182 and furnace-aged Inconel X-750, for which somewhat enhanced crack growth
rates were observed. However, the higher crack growth
rates were statistically significant only for the Inconel
182 specimen, and only a single specimen had been
tested.

6. Chemical deaning of steam generators


6.1. Description of the chemical cleaning process

The performance and operating life of a number of


PWR steam generators has been adversely affected by
the accumulation of corrosion products on the sec-

D.R. Diercks / Effect of decontamination on aging processes

ondary side [38]. These corrosion products form primarily as a result of impurity ingress owing to condenser
in-leakage and can seriously damage steam generator
components. Feed train corrosion products enter the
steam generator as particulates (typically Fe and Cu
corrosion products) or as dissolved ions. In the steam
generator, they react chemically or agglomerate to form
sludge deposits on the tube surfaces and tube support
system. These deposits, in turn, impair heat transfer and
form effective sites for localized corrosion. A related
problem occurs at carbon steel tube support plates,
where the accumulation of corrosion products can cause
deformation (denting) of the steam generator tubes. In
some severe cases, these corrosion phenomena have
necessitated total replacement of steam generators.
Mechanical methods for sludge removal from PWR
steam generators have not proven entirely satisfactory,
and alternative chemical cleaning methods are of considerable interest. The Steam Generators Owners Group
(SGOG), under EPRI sponsorship, has conducted research on this problem for approximately the past 10
years [39,40]. As a result of this effort, non-proprietary
chemical solutions utilizing EDTA (diammonium salt),
i.e. E D T A - ( N H 4 ) 2 , as the active ingredient have been
developed for the removal of iron- and copper-bearing
sludge deposits.
6.2. Corrosion studies on chemical cleaning

Extensive demonstration and qualification tests were


conducted in the course of developing the chemical
cleaning solutions. Initial tests conducted by various
laboratories [39-41] determined thai the solutions were
effective in removing accumulated corrosion products
from steam generators, and no corrosion problems were
encountered, aside from two undesirable side-effects.
The first of these was the occurrence of preferential
corrosion of carbon and alloy steel weld regions, with
the extent of this corrosion being unacceptable under
some of the conditions evaluated. The second undesirable side-effect was the retention of sulfur-bearing residues on steam generator surfaces after cleaning. Extensive laboratory tests were conducted under EPRI
sponsorship to evaluate both of these side-effects, as
summarized here.
The weld region corrosion testing program was conducted utilizing potentiodynamic polarization techniques and more elaborate electrochemical tests on
mocked-up PWR steam generator geometries consisting
of Inconel 600 tube bundles and carbon steel weld
blocks [41,42]. These tests found that the chemical
cleaning of steam generators using the generic SGOG

215

magnetite solvent can be carried out without causing


unacceptable levels of weld region corrosion, although
no materials subjected to long-term aging were tested.
Because of differences in sludge composition and steam
generator geometry and materials, site-specific qualification tests are recommended before chemical cleaning
is applied to particular steam generator.
The possible deleterious effects of the sulfur residue
remaining on steam generator surfaces after chemical
cleaning were also investigated [43]. The principal source
of the sulfur residue is the corrosion inhibitor present in
the chemical cleaning solutions, and its presence may
lead to accelerated localized corrosion of the tubing. In
these investigations, Incoloy 600 tubing specimens in
the non-flawed and flawed conditions were exposed to
the generic SGOG chemical cleaning processes in order
to produce representative sulfur residues on their
surfaces. These residues were characterized with respect
to their chemical state and morphology by using several
metallurgical analysis techniques. Selected specimens
were then exposed to typical and 'worst-case" wet layup
and operational conditions and evaluated for evidence
of accelerated corrosion. No initiation of new flaws or
propagation of existing flaws was observed under any of
the test conditions, with the exception of one control
(not chemically cleaned) stressed-strip specimen from
the SGOG guidelines operational test, which exhibited
IGSCC. In all cases, the inventory of sulfur added to
the system by chemical cleaning was found to be small
compared to typical sulfur ingress into the steam generator during normal operation. It was concluded that the
chemical cleaning residue does not cause increased susceptibility of Inconel 600 steam generator tubing to
localized corrosion, and no further experimental work
was recommended.

7. Potential interactions between decontamination and


aging
7.1. Areas of concern

A large number of nuclear reactor components will


be subjected to multiple chemical decontaminations or
chemical cleanings over their normal 40-year service
life. Many of these components will simultaneously
undergo one or more of the metallurgical aging processes
described previously. Since these aging processes can
increase the susceptibility of the materials of construction to corrosive attack, the possible adverse interactions of decontamination and aging must be considered
in licensing nuclear plants for extended life operation.

216

D.R. Diercks / Effect of decontamination on aging processes

Based upon the results of corrosion experiments


conducted with the CAN-DECON, LOMI, and SGOG
chemical cleaning processes discussed above, two broad
areas of concern with respect to aged materials are
identified here. The first area, possible non-uniform
corrosive attack of aged material, encompasses a variety
of localized corrosion processes that may be enhanced
by metallurgical aging and exposure time under LWR
operating conditions. The second potential problem area
relates specifically to in-core and near-core components,
which are not yet routinely exposed to decontamination
solutions in the United States.

7.1.1. Non-uniform corrosive attack of aged material

The CAN-DECON process can produce non-uniform corrosive surface attack, including I G A and pitting, under at least some conditions in sensitized type
304 SS, sensitized Inconel 600, and tempered Inconel
X-750. In the case of sensitized type 304 SS, the observed I G A has been linked to subsequent enhanced
IGSCC. Minor pitting of sensitized Inconel 600 has also
been observed after N P / L O M I and A P / L O M I treatment. Such non-uniform attack is of concern because it
creates sites for subsequent SCC or, in extreme cases,
may of itself lead to significant penetration.
None of the tests described above was carried out on
material subjected to prior long-term aging, where lowtemperature sensitization and related precipitation phenomena may further facilitate non-uniform corrosion.
In addition, Inconel 82 and 182 weld filler metals have
not been thoroughly tests for non-uniform corrosion
effects, and no tests have been conducted on the cast
duplex stainless steels. The latter alloys are suspect
because their duplex austenite-ferrite microstructure
creates the potential for differential corrosion rates of
the two phases or accelerated attack at the phase
boundaries through galvanic effects. These concerns are
supported by corrosion studies showing that the ferritic
stainless steels typically have significantly higher general corrosion rates than the austenitic stainless steels in
decontamination solvents.
The carbon and low-alloy steels are not, in general,
susceptible to I G and SCC in LWR environments.
However, a number of carbon and low-alloy steels have
exhibited significant general corrosion rates in the
CAN-DECON LND-101A reagent and, to a lesser extent, in the NP-LOMI and AP-LOMI solutions. In
LWR systems commonly subject to chemical decontamination, these alloys, when present, are frequently clad with a more corrosion-resistant alloy. This
creates the possibility for accelerated localized corrosion

of the carbon or low-alloy steel underclad at locations


where cracks or other flaws have penetrated the clad.
For this reason, these alloys are included for consideration here.

7.1.2. Corrosion concerns reading to core decontamination

The decontamination of LWR cores and adjacent


internal components would expose several other structural alloys to decontamination solutions and would
raise additional concerns with respect to corrosion. The
additional alloys exposed include high-strength Ni-based
alloys such as Inconel 625 and Inconel 718, the
Zircaloy-2 and -4 fuel cladding, and Co-based were-resistant alloys used on control rod drives. Limited corrosion data on some of these alloys in selected decontamination solutions and the small amount of available
experience from core decontaminations generally indicate no serious compatibility problems. However, additional site-specific qualification tests would clearly be
required before core decontaminations could be carried
out on a routine basis.
Another concern with core decontamination is the
possibility that contact with the decontamination solutions may further promote irradiation-assisted IGSCC
in BWR components. No data are available on this
possible interaction, but the I G A produced in sensitized
type 304 stainless steel by some decontamination treatments reinforces this concern.

8. Summary
In summary, experimental data and experience with
the chemical decontamination and chemical cleaning of
nuclear reactor components indicate no severe materials
corrosion problems that would preclude the use of these
techniques. However, no data are available on materials
subjected to prior long-term aging, and concerns exist in
several areas, particularly with respect to aged materials. These areas of concern include: (1) possible enhanced pitting, IGA, and I(3SCC in aged alloys; (2)
non-uniform corrosion effects in aged case duplex stainless steel; (3) possible unacceptable general corrosion
rates of carbon and low-alloy steels; (4) localized corrosion at flaws in clad carbon and low-alloy steels; (5)
possible enhanced irradiation-assisted IGSCC in aged
BWR core components; and (6) the limited corrosion
data available on the high-strength Ni-based and other
alloys used for core structural applications.

D.R. Diercks / Effect of decontamination on aging processes


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