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Guideline for the Development of

High Quality Stress Corrosion Crack


Growth Data

NULIFE (07)21 June 2008


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Distribution List

NULIFE Participants EG1 Materials and RA3 SCC

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CONTENTS

1 Introduction 7

2 SCC test guideline 8


2.1 SPECIMEN MACHINING 8
2.2 TEST MATERIAL 8
2.3 ENVIRONMENT 9
2.4 CRACK MONITORING 10
2.5 INSTRUMENTATION 10
2.6 ASSEMBLING 10
2.7 TESTING PROCEDURE 11
2.8 EVALUATION 13

3 Reporting recommendations 17
3.1 INTRODUCTION/BACKGROUND 17
3.2 EXPERIMENTAL 17
3.3 MATERIAL 18
3.4 SPECIMENS 19
3.5 ENVIRONMNET 20
3.6 EXPOSURE 21
3.7 POST TEST EXAMINATION 21
3.8 EVALUATION 21
3.9 CONCLUSIONS 22
3.10 ACKNOWLEDGEMENTS 22
3.11 OTHERS 23

4 References 24

Appendices
A Checklist before start of test
B Reporting table headings

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1 INTRODUCTION
This paper is a proposal for a “European guideline” on crack growth measurements
concerning stress corrosion cracking (SCC). The basis of the paper is 20 years of experience
at Studsvik on crack growth measurements in simulated LWR environments. Information is
also collected from [1- 5] as well as experiences within the participants in pilot project RA-3
on stress corrosion cracking. Also included in this paper is a list recommendations what ought
to be included in a crack growth report.

The background to the present guideline is the large scatter in data observed between
laboratories, even when the same heat is tested. Particularly weld materials, e.g. Alloy 182
display a large scatter. Some possible factors that contribute to the differences were identified
in the test protocol for a Round Robin on Nickel Alloys 600 & 182 [1]:
1. Specimen machining technique, which may create pre-cracking problems and/or
subsequent crack front unevenness.
2. Pre-cracking technique, including sequence of loading conditions and extent of the
crack advance in each phase.
3. SCC transitioning technique, including the sequence of loading conditions and the
extent of crack advance in each transitioning phase.
4. Water chemistry controls, especially stability and purity of outlet conductivity and O2
concentration.
5. Stability of temperature during testing.
6. Stability of loading, including load applied by the servo-testing machine as well as
indirect load fluctuations by system pressure fluctuations. “Noise” from dual stage
hydraulic servo valves and ≈ 1 Hz fluctuations in system pressure from the high
pressure positive displacement pump (which act on area of the loading linkage at the
autoclave pressure seal) are of particular concern. Evidence of very high growth rate
response in high yield strength materials during loading fluctuations makes this a
critical area.

The recommendations in this guideline are divided in sections structured according to the
normal sequence of events of a CGR test. It is very difficult to present a general guideline
because the object of different tests may differ, and all aspects cannot be covered in this
paper. In addition, there is no standard available for stress corrosion crack growth rate testing.
However, selected parts from ASTM E399 (fracture toughness) and E647 (fatigue) are
normally used when applicable

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2 SCC TEST GUIDELINE
The following headlines cover the most important sequences in a normal crack growth
measurement in simulated LWR environment. The sections are listed in the order of a normal
sequence in a CGR test, in each section the most important issues are discussed and a list of
recommendations presented.

2.1 SPECIMEN MACHINING


When compact tension (CT) specimens are used the following recommendations are to be
considered:
• Specimen dimensions are recommended in ASTM E399, E647 and E1820. The
specimen length is often twice the size of the width (note that this is outside the
recommendation in E647).
• The machining of side grooves (SG), 5% of specimen thickness on each side to assure
a straight crack front. The SG should be machined without cold work deformation on
the surface to avoid crack initiation from the bottom of the SG during the test, i.e. by
EDM (Electron discharge machined). Especially austenitic steels are sensitive to
influences of work hardening. The melted zone on the specimen surface caused by
EDM should be removed, i.e. by polishing.
• Fatigue pre-cracking should be performed prior to the test, either in air or in situ. In
ASTM E399 and E647 recommendations are given which control the length and
straightness of the crack front. The stress intensity, K, should be below the maximum
K in the test.
• Critical specimen dimensions should be documented.

2.2 TEST MATERIAL


The following documentation regarding the test material should be available and reported:
• Acceptance certificate (heat, tensile properties, chemical composition)
• WPS (welding procedure specification) for weld material
• Material condition during test (i.e. as welded, heat treatment, cold work, irradiation
etc.)
• Neutron fluence for irradiated material (irradiation condition, spectrum, temperature
etc.)
• Tensile properties, preferably at both room temperature and at testing temperature
• Microstructure characterisation, i.e. grain size distribution, grain size, typical particles.
• References to similar tests where the same heat has been tested

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2.3 ENVIRONMENT
When boiling water reactor (BWR) environment is simulated:
• For normal water chemistry (NWC) nothing but oxygen (or hydrogen peroxide) is
added to pure water. The amount may differ between tests, however the difference
between inlet and outlet oxygen content should be less than 20 %.
• For hydrogen water chemistry (HWC) hydrogen or very low amounts of oxygen is
added to pure water.
• To ensure that NWC or HWC is achieved the corrosion potential (ECP) on the
specimen is measured. A reference electrode is placed as close as possible to the
specimen, i.e. within 25 to 50 mm or closer if the specimen is not electrically isolated
from the loading linkage.
• The conductivity should be monitored continuously at least on the outlet water, the
outlet conductivity should be within 1.5 times the inlet conductivity. For “high purity”
water an outlet conductivity of 0.1 µS/cm is desirable and achievable for oxygen
contents less than 2 ppm. Abnormal values or transitions should be explained (i.e.
impurities, technical difficulties or corrosion products).
• The pure degassed inlet water should be checked for bacteria, organics, TOC and other
impurities and minerals. The conductivity should not exceed 0.07 µS/cm.
• Temperature measured continuously and controlled within ± 1 °C
• Pressure monitoring, the system fluctuations caused by the high pressure pump should
be diminished using a pulse dampener (accumulator). Typical values on the short term
fluctuations were reported in [3] and did not exceed 0.2 MPa.
• Flow rate monitoring, the flow rate should be sufficient to refresh the autoclave
volume in one to three hours.
• Control of the anion concentration in the outlet water, continuously or by grab
samples. Grab samples should be made on a regular basis as needed to reflect
significant variations in water chemistry. Anion levels (SO42-, Cl-, and F-) below 5 ppb
are desirable in “high purity” water [10].

For simulated primary water reactor (PWR):


• PWR is simulated by addition of boron, lithium and hydrogen to pure water.
• For a once-through autoclave system the environment is controlled during the test by
measuring the conductivity continuously in the outlet water and compared with the
theoretical target value.
• When a recirculation system is used the amount of Boron and Lithium may be
controlled by other techniques, i.e. saturation of the ion exchanger.
• The pure degassed inlet water should be controlled for bacteria, organics, TOC and
other impurities and minerals.
• Temperature measured continuously and controlled within ± 1 °C
• Pressure monitoring, the system fluctuations caused by the high pressure pump should
be diminished using a pulse dampener (accumulator)
• The flow rate sufficient to circulate the water and the actual flow rate should be
reported.

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• On a regular basis (once a week) a grab sample of the outlet water to control and
document the amount of impurities (SO42-, Cl-, F-). Maximum values are controlled in
guidelines (i.e. chemistry water guideline). Also the amount of B and Li is controlled
in these samples.
• The hydrogen content is measured continuously on the outlet water. If not possible,
grab samples are taken at least once a week to measure the concentration.

2.4 CRACK MONITORING


A direct current potential drop (DCPD) system is recommended for monitoring the crack
growth. However, other techniques are also possible (ACPD, acoustic emission etc.).
• The current and potential wires should be made of a low resistant material. Avoid
combining more materials than necessary. Also, the weld ability of the material should
ne noticed.
o The current wires are typically made of Nickel or Platinum.
o The potential wires are typically made of Platinum or the testing material.
• The current through the specimen should be shifted every 10 second or so to
compensate for thermoelectric effects.
• Make sure the current and potential wires are isolated from the autoclave and loading
clevises.
• The potential drop is then converted to crack length using for example a calibration
curve for the specific specimen dimension or by Johnson’s formula.

2.5 INSTRUMENTATION
Be sure to use a calibrated data acquisition system which meets the demands for the
measurement (resolution, stability etc).

2.6 ASSEMBLING
Prior assembling the Specimen in the testing machine:
• Check that the load train is aligned
• Check that the load cell is balanced
• Clean the specimen (e.g., ultrasonic in acetone and ethanol) prior to mounting it in the
autoclave

Different testing machines or loading devices are possible (servo hydraulic, servo electric,
electric motor etc.). Check that the machine capacity satisfies the testing requirements
(frequency, maximum load etc.).

When assembling the specimen:

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• If a reference electrode is used, keep the distance between specimen and electrode as
short as possible (within 25-50 mm).
• Some nickel base alloys tend to shift in resistivity during time at LWR temperatures.
If the DCPD technique is used, this change in resistivity will result in apparent crack
growth. A reference piece should be made from the same heat and condition as the
specimen to compensate for resistivity changes. Alternatively an additional pair of
potential leads can be mounted on the back of the specimen.
• The specimen must be electrically isolated from the autoclave.

2.7 TESTING PROCEDURE


Different kind of loading technique may be used in different tests, i.e. constant load, constant
displacement or constant K. The maximum value of stress intensity is defined in ASTM E399
and E647 using the specimen size criteria based on the yield strength, ultimate strength or
combination of both. Since there are no standard for SCC testing the K validity are somewhat
uncertain and may differ between different materials and heats. For unirradiated, non cold
worked or precipitation hardening (PH) material ASTM E399 is recommended with the
specimen size criteria based on the flow stress (average of yield and ultimate strengths) [5].
For cold worked and PH material ASTM E399 using the yield strength criteria is more
applicable. For irradiated material ASTM E399 is preferred using the difference of irradiated
and unirradiated yield strength divided by two plus the yield strength of the unirradiated
material (see Equation 1).

YSirr − YSunirr
YSeff = + YSunirr Equation 1
2

The factor 2 in the denominator may increase to a factor of 3 if the tested material has a high
dose [5, 6]. Tests performed on unirradiated sensitized stainless steel in Studsvik have shown
that ASTM E647 resulted in relevant data when the flow strength criterion is used [7, 8].

What kind of testing procedure to use for a specific test depends on many things, i.e. material,
purpose of test, testing machine capability etc. Here are two different procedures presented,
both typical for SCC tests. However, there probably exist many more variants of SCC testing
procedures.

Procedure 1:
• After assembling the specimen (and reference piece and reference electrode if
needed), the internals are photographed from several angles to show the location of
all internals and parts (if they not already are documented).
• A checklist should be filled in before the autoclave is closed. An example of such
a checklist is presented in Appendix A.
• The system is closed and (for BWR tests) high purity water containing O2 will be
flowed through the system at an appropriate pressure. For PWR tests, water
containing B as H3BO3 and Li as LiOH with H2 will be flowed for one day or

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more, depending on the time which is needed to achieve the desired outlet
conductivity (≤ 0.1 µS/cm for BWR testing). Continuous digital records of inlet
and outlet conductivity should be kept (inlet or outlet is adequate for PWR
testing).
• The autoclave is then heated with the specimen at low load or unloaded to the
target temperature. Again the specimen should be allowed one day or more to
conditioning to the new environment and the outlet water chemistry should be
stabilised. For BWR environment the specimen should remain unloaded for at
least a week while the specimen is pre-oxidised and ECP become reasonable
stable, the drift in ECP should be less than 10 mV SHE per day. However, for ECP
to reach steady state may take many 1000 hours. Continuous digital records of
inlet and outlet conductivity will be kept, before, during and after the test.
• The specimen is then be loaded to 0.8*Pmax, and the dc potential drop system
equilibrated for several hours. The specimen is then loaded according to table 1.
Digital data of all test parameters must be recorded, and any problem carefully
noted (overloads, system trips in load or temperature, flow rate fluctuations, water
chemistry fluctuations). If crack arrest occurs for a week at any stage in steps 1 – 9
(or more than 2 weeks at constant load) go back in the sequence to the next most
aggressive loading condition.

Table 1
Step Kmax, Pmax Load ratio, R Frequency Crack increment
Parts of max a/W
1 0.8 0.3 1 Hz sine 0.01
2 0.9 0.5 1 Hz sine 0.006
3 1 0.6 1 Hz sine 0.006
4 1 0.7 1 Hz sine 0.006
5 1 0.7 0.1 Hz sine 0.004
6 1 0.7 0.01 Hz sine 0.004
7 1 0.7 0.001 Hz triangle 0.004
8 1 0.7 0.001 Hz + 9ks hold 0.002
9 1 1 Constant ≥1 months
10 1 0.7 0.001 Hz + 9ks hold ≥0.002 & ≥2 wks
11 1 1 Constant ≥1 months

• When using a reference electrode it is desirable to investigate if the current


switching of the DCPD measurement affects the corrosion potential. In order to
check this, a separate high impedance voltmeter (electrometer) can be used to
measure the potential between the specimen and the reference electrode while the
DCPD measurement is still operating. The so measured corrosion potential should
be unaffected by the current switching.
• At the end of the test the load should be removed from the load train and the tare
load of the load cell reported (load cells do not always return to zero after several
months of use). If the tare load is sufficient the stress intensity in the specimen has

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to be corrected. After that the system is cooled down. The specimen should be
photographed, then air fatigue cracked to failure using initially the same Kmax and
R=0.1 at ≥ 1 Hz.

Procedure 2:
If table 2 is exchanging table 1 in the context above another useful procedure is presented.
This one may be used when the testing material is relatively sensitive to SCC and/or the
testing machine cannot fulfil the requirement of all the steps. The specimen is now loaded
with a low frequency cycling load, the frequency may depends on the testing machine. At step
2 a hold time at maximum load is introduced and through steps 3 to 4 the hold time is
increased in steps subsequent to the constant loading condition in step 5.

This method has successfully resulted in intergranular cracking in many different materials
and heats in various tests.

Table 2
Step Kmax, Pmax Load ratio, R Frequency Crack increment
Parts of max a/W
1 1 0.7 0.05 Hz triangle 0,006
2 1 0.7 0.05 Hz + thold=100 s 0.004
3 1 0.7 0.05 Hz + thold=1000 s 0.004
4 1 0.7 0.05 Hz + thold=9000 s 0.002
5 1 1 Constant ≥1 months

The presented procedures above may, of coarse, need to be modified to satisfy the objectives
of a specific test. Also, for very low values of stress intensities the load ratio may needs to be
decreased from 0.7 to 0.6 or lower to achieve a ∆K sufficient for a crack to grow. The crack
increments in Table 1 and 2 may be adjusted to achieve at least 10 times the crack
measurement resolution to ensure “hard data”. However, for low CGRs the duration of the
test would be very long using any of the criteria and shorter increments may be necessary.

2.8 EVALUATION
First the specimens fracture surface is photographed by a camera with sufficient
magnification and quality that the details of the (oxidized) crack and crack front are clear (i.e.
so the specimen occupies nearly the full image). The fracture surfaces can then be cleaned in
an ultrasonic bath in distilled water for about 10 minutes and rinsed in acetone prior to SEM
examination. SEM examination should include a low magnification photo (or montage) of the
entire oxidized fracture surface (pre-crack and SCC region), as well as higher magnification
photos of the pre-cracking and especially the SCC regions.

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A connection between local microstructures and the respective local crack growth should be
investigated during post-test investigation, i.e. by investigating cross-sections of the fracture
surface in light optical microscope.

If the crack front is reasonably uniform the crack length can be determined by measuring the
crack length at 20 equidistant points along the specimen thickness. The true crack length can
then be calculated by averaging the 20 data points. However, if the percent of engagement (%
of the crack front with SCC) is low the evaluation becomes more complicated and other
methods may be required.

EPRI’s material reliable project (MRP) gives recommendations concerning evaluation on Ni-
based alloys [4]. Especially Ni-base weld materials often show local crack growth with quite
low percent of engagement. Some important recommendations listed from MRP:
• At least 50% engagement
• An average crack length of at least 0.5 mm
• CGR based on average crack length rather than maximum crack length so that local
areas with higher growth rates become less significant
• Average crack length based on representative areas, area with no or limited crack
growth is disregarded.

The information from the fractographic investigation can then be used to correct the crack
growth data estimated by DCPD. In the context that follows a linear correction of the DCPD-
data is described. However, other procedures are possible (i.e. nonlinear) and depending of
the objectives of the test no correction at all may by the most suitable. A schematic illustration
of the procedure is presented in Figure 1. After testing, the primary crack length versus time
curve from the DCPD measurements (curve 1 in Figure 1) is adjusted to fit with the data from
the fractographic examination. This is done by correcting each data point of the DCPD curve
with a factor, such that the curve fit the correct start and final crack lengths (curve 2 in Figure
1). The correction factor was obtained by the ratio of the linear slopes of the DCPD curve and
the correct start and final crack lengths. The following expression is used to linearly correct
DCPD data:

a corr = CF ⋅ ( a DCPD − a start ) + a start


true
Equation 2

where CF is the correction factor, acorr is the linearly corrected crack length, aDCPD the crack
length estimated by DCPD, and astart and astop the DCPD estimates of the start and final crack
lengths, respectively. See also Figure 1 for more explanations.

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Figure 1
Schematic illustration of how the crack length versus time curve from the DCPD
measurement was linearly corrected to account for the crack length measured on the fracture
surface.

In this way the average CGRs of the test specimens can be calculated assuming relatively
planar cracks and fairly even crack fronts. However, in case of testing of weld materials or
irradiated specimens (especially when testing HAZ) uneven and rugged crack increment areas
can be formed complicating the evaluation.

There are two basic ways of CGR determination: (i) calculation of average values based on
post-test measurement of fracture surface and (ii) numerical derivation of the corrected crack
length vs. time experimental data curve. The first way is used if the load and chemistry
regimes were stable during the whole test or when visible marks could be found on the
fracture surface. The second one is used if regimes are changed during the test and no
detectable marking on the fracture. Of course, both methods may be used if possible.

Before classify a test as not valid it is recommended to use an additional way of CGR
calculation for the specimens. CGR calculation only in the specimen areas where the crack
shows relatively straight growth not affected by constraint of the other parts of specimens,
respective parallel cracks. The average and maximum CGR can be calculated from the
average and maximum crack increment in the selected areas. The local values could give an
idea about local CGR ranging in the material in connection to a local microstructure variance.
As it is known EAC cracking is very local process and especially in a complex microstructure
it would be conductive to apply a local approach. Usually the difference between the local
average and the local maximum CGR values is not significant in comparison to the average
CGR values over the specimen thickness.

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The real stress intensity during the test can then be calculated based on the corrected crack
length versus time curve and load data from the test.

According the standards (ASTM E399, E813, and E1820) to ensure validity of K the crack
extension should lie in a plane slope of which not exceeds an angle 5 - 10° from the plane of
the notch and the difference in crack lengths inside the specimen does not exceed 5% of
specimen width W see also. The restrictions were set because of every local inclination of the
fracture path from the notch plane means local mixed mode loading (mode I and II). Then K
applied externally is higher than K acting locally and in fact, determining the local cracking
process in the material. For example in case of local crack plane inclinations due to
intergranular fracture in a coarse grain material the local K values controlling the growth can
differ nearly by 50% from the applied KI as been calculated [9], see Fig. 2. Similar effect to a
significant divergence between local K value and the applied K would have any significant
step of the crack front.

0.9

0.8

0.7

0.6
Keff / KI

0.5 CrackCrack
frontbranching
step
0.4

0.3

0.2

0.1

0
0 50 100 150 200 250 300
Aus tenitic grain s ize [µm]

Figure 2
The full line shows calculated relationship of local effective Keff and applied KI for
intergranular fracture in A316 austenitic steel. Dashed lines show effect of a crack front step,
as on right in 1T CT, on the relationship (arrow marks the crack direction) [9].

Therefore any violation of the standards requirements on the crack path flatness and the crack
front straightness brings a certain level of indefinites of the acting K. The level of indefinites
is not negligible even for common intergranular fracture.

Evidently, only an effective K factor can be assumed for the complex fracture path specimens.
For purpose of a disposition line determination the effective K values can be calculated
according standards formulas using the corrected crack lengths and load data from the test.

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3 REPORTING RECOMMENDATIONS
This chapter presents a list of what should, respectively ought to be included in a report
concerning a crack growth measurement. It is important the test results fulfill the
requirements from present as well as future demands.

Avoid unnecessary data in the report context. Put the information (fractography, material
characterization, diagrams etc.) in suitable appendices.

The following headlines are an attempt, based from a normal SCC test report structure, to list
the demands and recommendations.

A format for data reporting is given in appendix B.

3.1 INTRODUCTION/BACKGROUND

Should be included:
o Why the test is performed – the object of the test.
o References to previous similar tests.

Ought to be included:
• Put the test in an international perspective.
• Published and relevant data.

3.2 EXPERIMENTAL

Should be included:
o Description of the equipments used
o Description of the measurement techniques used
o The nominal test environment(s)
o Autoclave volume.
o Testing procedure, i.e. constant load, constant stress intensity, constant displacement,
periodic partial unloading.

Ought to be included:
• Internal identification of test equipment.

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3.3 MATERIAL
3.3.1 Rolled or wrought materials

Should be included:
o Internal identification of the material.
o External material identification, i.e. AISI 304 or Alloy 690.
o Chemical analysis and tensile properties, i.e. from the material certificate.
o Picture of the microstructure (could be combined with LOM at the post test
examination).
o Heat treatment or other treatment if any (sensitization, cold work, irradiation etc.).
o Tensile properties representative to the testing temperature (including stress and strain
curves if available)
o Copy of the heat certificate from the manufacturer if available.

Ought to be included:
• If possible chemical control analysis.
• Grain size and micro hardness.
• Manufacturer, product form, thickness (normally included in the heat certificate).

3.3.2 Welds

Note that the analysis and tensile properties of a weld material not is the same as the filler
metal/welding electrode. Also, it varies between different welding layers because the first
strings will have more influence from the admixture of the base metal while the last strings
mainly are filler metal. Further, the thermal process varies between different strings.

Should be included:
o Internal identification of the material.
o External material identification, i.e. Alloy 182.
o Picture of the microstructure (could be combined with LOM at the post test
examination).
o Heat treatment or other treatment if any (sensitization, cold work, irradiation etc.).
o Tensile properties representative to the testing temperature (including stress and strain
curves if available).

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o Overview showing where in the weld the crack will propagate and the crack direction
relative to the weld strings/dendrites.
o Documentation from the welding wire manufacturer and welding company, such as
certificate for ground material, filler metal and WPS (welding procedure
specification).
o If possible chemical control analysis from a relevant part of the weld or machined
specimen.
○ Ferrite content for stainless steel weld metal.

3.3.3 Other materials (Cast)

○ Relevant information regarding forging and weld metal.


o Ferrite content and casting method.

3.4 SPECIMENS

Should be included:
o Type of specimen (CT, SENB, etc) and critical dimensions.
o Drawing or schematic of the specimen.
o Position of the machined specimen relative to the material.
o Direction of the specimen relative to the rolling or dendrite direction.
o If side grooves is used this should be noticed together with depth, radii, manufacturing
procedure and if the side grooves were manufactured before or after the fatigue
precracking.
o Deviations from the standards of the specific specimen type if any.
o Relevant information about the precracking (i.e. maximum stress intensity), evaluate
da/dN if needed.
o Estimate the validity of the specimen after precracking, before the specimen is
mounted in the autoclave. Criteria, crack length, obliquity (visible inspection of the
specimen edges) etc.
o After post test examination, estimate the validity of the specimen using the load data
and crack length together with appropriate standard (i.e. ASTM E399, ASTM E647).
o Specimen manufacturer.
o How the specimen was machined (Milled, EDM etc.).
o If necessary a dimension protocol for the specimen.

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3.5 ENVIRONMENT
3.5.1 BWR

Should be included:
o Relevant temperature measurements.
o Inlet and outlet conductivity.
o Oxygen content in at least outlet water and if possible also in outlet water.
o Levels of impurities (sulfate, fluoride and chloride), if necessary (i.e. transient) control
the water for other elements.
o Corrosion potential measured on the specimen.
o Flow rate.
o Levels of intended impurities if any (H2, sulfate etc).
o Autoclave pressure

Ought to be included:
• TOC if needed
• Deviation of the measured parameters, i.e. standard deviation.
.
3.5.2 PWR

Should be included:
o Relevant temperature measurements.
o Regular analysis of the outlet water (B and Li).
o pH300°C if different environments were included in the test.
o Regular analysis of the impurities (SO42- and Cl-).
o Regular analysis of the hydrogen content.
o Flow rate.
o Conductivity
o Autoclave pressure

Ought to be included:
• Partial pressure of hydrogen if different hydrogen contents or temperatures were
included in the test.

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• Deviation of the measured parameters, i.e. standard deviation.

3.6 EXPOSURE

Should be included:
o Duration (h).
o Important events during the test.
o Deviations and how they influenced the test.

3.7 POST TEST EXAMINATION

Should be included:
o Fractography (i.e. overview and details) including direction of crack propagation.
o References in the overview where the details are located.
o In case for unirradiated specimens: metallography (LOM). At least one cut should be
made perpendicular to the crack plane in a representative specimen, if many are tested.
The picture should show how the crack is located according to the microstructure.
This could be combined with the material characterization, see section 3.3.1.
o Documentation showing if the crack growth was even distributed over the width of the
specimen or if the growth only was local (picture, drawing, measure of deviation etc.)
o Investigation of the microstructure in the side grooves if motivated (i.e. crack growth
from the bottom of the side grooves).
o Collage of SEM-images in a suitable magnification showing the fatigue pre crack,
EAC and post fatigue.
o Measurements data from the determination of actual crack length, i.e. in a table or
figure, preferable located in the appendices.

3.8 EVALUATION

Should be included:
o Diagrams of load, stress intensity and crack length as a function of time (one diagram
for the whole test, details are included if needed).
o Time increment for the determination of crack growth rates and a motivation of the
increment used.

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o The crack length determined from the fractography. The length of the precrack should
also be given. The method used to determine crack lengths should be described.
o Crack growth rates and a description of the method(s) used in the evaluation.
o Estimation of the error in DCPD measurement, deviations should be explained.
o A description how the DCPD measurement was corrected from the actual crack
lengths determined from the fractography.
o r2-value (regression coefficient) from the linear adjustment of DCPD data.
o The stress intensity, and the variations, during the test.
o dK/da, if needed.
o For weld metals the maximum and average crack lengths.
o For weld metals amax/aaverage.
o ”Percentage of engagement”.
o Fulfilment of criteria for the specific standard regarding crack front (before and after
the test), stress intensity etc.
o If several distinguished steps have been performed (also gentle cycling) on the same
specimen the following parameters should be reported for each step: ∆t, ∆a, K and r2.
o Detailed data on the crack growth measurements should be reported in a table located
in the appendices.

Ought to be included:
• Observations that may have influenced the test.
• Judgment of the contribution from cyclic loading or partial unloadings if applicable
(∆atot=∆af(N)+∆af(t)).
• Transients that may have influenced the crack growth.
• Quality number Q (∆a⋅∆t). Q>10 may be regarded as “hard data”.

3.9 CONCLUSIONS
o The project conclusions are summarized
o Achievement of objectives.

3.10 ACKNOWLEDGEMENTS
Don’t forget to mention those who contributed to the accomplishment and discussions. In
most cases is it not only the author(s) who deserve the credits for a good work.

NULIFE (07) 21 Page 22 of 26


3.11 OTHERS
• Lessons learned

NULIFE (07) 21 Page 23 of 26


4 REFERENCES
[1] Personal contact with Peter Andresen (2007), GE-GRC, USA
[2] Andresen, P.L. “SCC Testing and Data Quality Consideration”, Proc. Ninth Int.
Symp. on Environmental Degradation of Materials in Nuclear Power Systems -
Water Reactors, AIME, 1999
[3] Andresen, P. L. (1998). IGSCC Crack Propagation Rate Measurement in BWR
Environment, Executive Summary of a Round Robin Study. SKI Report 98:27,
ISSN 1104-1374.
[4] White, G, A et al. “SCC Development of Crack Growth Rate Disposition Curves for
Primary Water Stress Corrosion Cracking (PWSCC) of Alloy 82, 182 and 132
Weldment”, Proc. 12th Int. Symp. on Environmental Degradation of Materials in
Nuclear Power Systems - Water Reactors, AIME, 2005.
[5] P.L. Andresen, “K / Size Effects on SCC in Irradiated, Cold Worked and
Unirradiated Stainless steel”, Proc. 11th Int. Symp. on Environmental Degradation
of Materials in Nuclear Power Systems - Water Reactors, Stevenson, WA, 2003
[6] Jenssen, A et.al., “Crack Growth Behavior of irradiated Type 304L Stainless Steel in
Simulated BWR Environment”, Proc. 11th Int. Symp. on Environmental
Degradation of Materials in Nuclear Power Systems - Water Reactors, Stevenson,
WA, 2003
[7] Jenssen, A, Jansson, C and Sundberg, J. The Effect of Hold Time on the Crack
Growth Rate on Sensitized Stainless steel in High Temperature Water, Proc. 12th
Int. Symp. on Environmental Degradation of Materials in Nuclear Power Systems -
Water Reactors, AIME, 2005
[8] Jenssen, A, Efsing, P and Sundberg, J. Influence of Heat Treatment, Aging and
neutron irradiation on the fracture toughness and Crack Growth Rate in BWR
environments of Alloy X-750, Proc. 12th Int. Symp. on Environmental Degradation
of Materials in Nuclear Power Systems - Water Reactors, AIME, 2005.
[9] A. Brozova, J. Pokluda, “Effect of deformation rate on EAC of A316H and A321
steels in chloride solution“, Proc. Environmental Degradation of Engineering
Materials (EDEM), TU Gdansk and Bordeaux, Gdansk-Jurata, 1999, Vol. I, p. 151-
156.
[10] Efsing, P and Jansson, C. Screening of Crack Growth Data and the Relevance from
an End-User Perspective. 11th International Symposium in Environmentally assisted
Degradation of Materials in Nuclear Power Systems – Water Reactors, Stevenson
Washington, USA, 2003..

NULIFE (07) 21 Page 24 of 26


Appendix A
Checklist
Done? Preperations Notes Signature project manager
Known problems from previous tests reported?
Does the calibration time of the instruments cover the whole period of testing
Are the loadcell(s) calibrated and approved?
Are all pumps (high pressure as well as dosage) in good condition
Preperations of additatives/solutions
Manufacture of electrode
Inspection of valves and autoclave
Inventory of equipment
Inspection of oil and filter of the testing machine
Inspection of servovalves if a servohydraulic testing machine is used

Done? Build up Notes


Correct material for DCPD wires
Are the wires mounted correct, marked and approved?
Specimen(s) pre fatigued and manufactured according to existing procedure?
Specimen(s) and load train alligned
Testing machine tuned (optimal PID), load cell balanced?
Isolation of specimen(s) and autoclave - measured and approved
Isolation (against specimen and autoclave) and position of electrode - measured
and approved
Specimen(s) photographed

Done? Pretest Notes


DCPD measurements in air performed with satisfying results?
DCPD resolution determined and approved?
Leakage in autoclave penetrations or sorrounding equipment?
Leakage observed in pumps?

NULIFE (07) 21 Page 25 of 26


Page 26 of 26 NULIFE (07) 21
Hardness
Type of loading
Partner
[%] A5test temperature
∆tRise [h]
Experiment (individual
Experiment

[%] Ztest temperature designation)


∆tHold [h]
[MPa]
Specimen code
∆tCycle [h]
Rm test temperature
[MPa]
Designation
∆tCL [h]
Rp test temperature
A525 °C [%]
Z25 °C [%] f [1/s] Material
Rm 25 °C [MPa]
R [-]
Rp [MPa] Type of material
25 °C
Material and specimen

1/2
Loading parameters

[µm]
dKI/dtRise [MPam /h]
Orientation
Mean grain size
Start 1/2
∆K [MPam ]
Microstructure
Al [wt.%]
Type of specimen
End
∆K [MPam 1/2]
Nb [wt%]
Ti [wt%]
Environm: BWR/PWR
KI,max Start [MPam 1/2]
Co [wt.%]
Cu [wt.%]
KI,max End [MPam1/2] T [°C]*
V [wt.%]
Mo [wt.%]
KI,i [MPam 1/2]
Cr [wt.%]
Ni [wt.%] Autocl. exch. rate [1/h]
S [wt.%] a/W [-]
P [wt.%] O2 in [ppb]*
Mn [wt.%] a [mm]
Si [wt.%]
O2 out [ppb]*
C [wt.%] <∆aCF> [mm]
PWHT/SR
Remarks <∆aSICC> [mm] in [ S/cm]*
Reports
<∆aSCC> [mm]
out [ S/cm]*
Material
Designation
N [-]
Crack growth data

pH in
∆a/∆N [µm/cycle]
pH out
da/dt [m/s]
Environmental parameters

Li content (as LiOH) [ppm]


da/dtinert [m/s]
da/dtRise [m/s] B content (as LB(OH)3) [ppm
Suggested reporting table headings for environment, loading conditions and material.
Appendix B

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