1 Introduction 7
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
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
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.).
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
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
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.
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:
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.
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.
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.
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.
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.
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).
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.
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.
3.6 EXPOSURE
Should be included:
o Duration (h).
o Important events during the test.
o Deviations and how they influenced the test.
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.
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.
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