Designation: E 453 – 79 (Reapproved 2001)

Standard Practice for

Examination of Fuel Element Cladding Including the
Determination of the Mechanical Properties1
This standard is issued under the fixed designation E 453; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope E 92 Test Method for Vickers Hardness of Metallic Mate-

1.1 This practice covers the procedures for postirradiation rials3
examination of cladding, determination of breached nuclear E 94 Guide for Radiographic Testing5
fuel elements, selection of material and tests for radiation E 112 Test Methods for Determining the Average Grain
studies, determination of radiation conditions, conduction of Size3
tests for mechanical properties of cladding, and the reporting of E 139 Practice for Conducting Creep, Creep-Rupture, and
data. Stress-Rupture Tests of Metallic Materials3
1.2 The purpose of this practice is to provide detailed E 146 Methods of Chemical Analysis of Zirconium and
guidelines for the postirradiation examination of fuel element Zirconium Alloys (Silicon, Hydrogen, and Copper)6
cladding and to achieve better correlation and interpretation of E 165 Test Method for Liquid Penetrant Examination5
the data in the field of radiation effects. E 261 Practice for Determining Neutron Fluence Rate, Flu-
1.3 This practice may be applied to metallic cladding from ence, and Spectra by Radioactivation Techniques7
all types of fuel elements. The tests described in this practice E 263 Test Method for Measuring Fast-Neutron Reaction
for determining mechanical properties of the fuel element Rates by Radioactivation of Iron7
cladding practice should be included in the preirradiation E 380 Practice for Use of the International System of Units
characterization of the cladding and for planning irradiation (SI) (the Modernized Metric System)8
effects tests for evaluation of materials for cladding and other E 466 Practice for Conducting Force Controlled Constant
components in nuclear reactors. Amplitude Axial Fatigue Tests of Metallic Materials3
E 606 Practice for Strain-Controlled Fatigue Testing3
NOTE 1—The values stated in SI units as described in Standard E 380 F 77 Test Method for Apparent Density of Ceramics for
are to be regarded as the standard.
Electron Device and Semiconductor Application9
2. Referenced Documents
3. Significance
2.1 ASTM Standards:
3.1 The physical and mechanical properties of cladding
B 353 Specification for Wrought Zirconium and Zirconium
materials can be altered by exposure to a high-energy neutron
Alloy Seamless and Welded Tubes for Nuclear Service
flux. The magnitude and relationship of these changes are
(Except Nuclear Fuel Cladding)2
functions of the material and its metallurgical condition; the
E 3 Methods of Preparation of Metallographic Specimens3
amount, rate, and energy spectrum of the radiation; the
E 8 Test Methods for Tension Testing of Metallic Materials3
exposure temperature; the test temperature; the purity, velocity,
E 12 Terminology Relating to Density and Specific Gravity
volume, and purification system of the coolant; and effects of
of Solids, Liquids, and Gases4
contained fuel.
E 21 Test Methods for Elevated Temperature Tension Tests
of Metallic Materials3 4. Determination of Radiation Conditions
E 45 Test Methods for Determining the Inclusion Content
4.1 Report all available data on the nuclear environment
of Steel3
including reactor operating history, reactor geometry, and
operating temperature. Provide neutron dosimetry for each
experiment (refer to Practice E 261 for applicable practices).
1
This practice is under the jurisdiction of ASTM CommitteeE10 on Nuclear Suggestions as a minimum guide in measuring the radiation
Technology and Applications and is the direct responsibility of Subcommittee
E10.02 on Behavior and Use of Nuclear Structural Materials.
5
Current edition approved Dec. 20, 1979. Published March 1980. Originally Annual Book of ASTM Standards, Vol 03.03.
6
published as E 453 – 72. Last previous edition E 453 – 72. Discontinued—see 1989 Annual Book of ASTM Standards, Vol 03.05.
2 7
Annual Book of ASTM Standards, Vol 02.04. Annual Book of ASTM Standards, Vol 12.02.
3 8
Annual Book of ASTM Standards, Vol 03.01. Annual Book of ASTM Standards, Vol 14.02.
4 9
Annual Book of ASTM Standards, Vol 15.05. Annual Book of ASTM Standards, Vol 15.02.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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environment are described in 4.1.1-4.1.5. to preserve its irradiated condition. Take special precautions to
4.1.1 Neutron Spectrum—For the particular facility utilized, ensure that the cleaning procedure does not entail high tem-
report the most complete neutron spectrum description avail- perature or high stress that might alter the as-irradiated
able from reactor physics computations, from preexperiment condition or state.
surveys, and from monitoring of the experiment. Calculate the 5.1.1.2 All tools selected for handling of irradiated fuel
neutron spectrum from suitable transport or diffusion theory elements should be of such a design and construction to
computer codes to best simulate the actual reactor conditions minimize the risk of accidental damage to the element. Do not
(that is, one-dimensional, cylindrical geometry, etc.). Report use elastomers and soft metals such as aluminum, copper, and
information on the neutron flux distribution versus neutron lead, in contact with the fuel element. During handling do not
energy. subject the fuel elements to any stresses for which they are not
4.1.2 Reactor Conditions—Report information on the local designed.
reactor operating time history and reactor geometry including 5.1.2 Shipping:
dimensions, materials, and locations. Obtain or calculate the 5.1.2.1 The shipping containers should be equipped with
number of equivalent full-power days (EFPD). suitable inserts, baskets, spacers, and supports so that the
4.1.3 Neutron Dosimetry—Determine the neutron fluence as surface of the element is not damaged during transit. Take
described in Practice E 261 and Test Method E 263. Normally, special care to avoid excessive vibration that can lead to
include the fast fluence above a given energy such as E > 0.1 fretting wear.
MeV or E > 1.0 MeV, the displacements per atom (dpa), and 5.1.2.2 It may be necessary to cool the fuel element during
reference the dpa technique used. For example, determine the shipment. If a coolant is not used, then calculations must show
fast fluence from the54Fe(n,p)54 Mn reaction in Zircaloyt10 or that the decay heat will not create an unacceptable increase in
stainless steel fuel cladding. In this case, accurate values of the the temperature of the fuel element.
iron content would be required, preferably preirradiation val- 5.1.3 Storage:
ues. Then, calculate the neutron fluence from a knowledge of 5.1.3.1 Observe the same precautions and procedures at the
induced activities, spectrum-averaged cross sections, and reac- receiving site as those observed at the shipping site.
tor operating time histories. 5.1.3.2 Storage facilities commensurate with the size and
4.1.4 Temperature Knowledge—For the evaluation of irra- mass of the fuel assemblies must be provided. The storage
diation effects on physical and mechanical properties, knowl- facility must have an environment that provides adequate
edge of the absolute irradiation temperature and its uncertainty cooling and protection to the element. For LWR fuel elements,
is extremely important. Where possible, use sufficient sensors demineralized water or air is adequate. Store LMFBR fuel
to provide a complete knowledge of the temperature pattern elements in an inert gas atmosphere or high-purity sodium.
throughout the assembly. When the use of sensors is not Moisture and oxygen can react with residual sodium and form
possible, state the method of determining the irradiation corrosion products on the LMFBR cladding. Avoid these
temperature. reactions, as they can lead to attack of the cladding, thereby
4.1.5 Irradiation Atmosphere or Medium—Report the com- destroying the as-irradiated surface condition.
position and impurities of the medium surrounding the speci- 5.1.4 Surface Preservation:
mens during irradiation in as much detail as practical. 5.1.4.1 In many postirradiation examinations, the surface of
4.1.6 Document the method of supporting/spacing, location the fuel element, including the corrosion film and crud depos-
of fuel rod, and pitch-to-diameter ratio. its, is of interest. Preserve these deposits as much as practicable
until the visual examinations are complete or until an adequate
5. Handling, Shipping, Storage, and Surface Preservation sample has been obtained.
5.1 It is essential that the conditions of the cladding caused 5.1.4.2 If the examination of loosely adherent surface de-
by irradiation and exposure to the operating environment be posits is of no interest, the deposits may be removed with a
preserved between the time the fuel element is discharged from soft-bristled brush. For LWR fuel elements, water or organic
the reactor and the nondestructive examinations are completed. solvents such as ethyl alcohol or acetone may be used as an aid
Overheating or even aging at the irradiation temperature during in removing loosely adhering deposits. For LMFBR fuel
handling and storage can result in partial annealing of the elements, avoid the use of water. Alcohol is a suitable solvent
radiation effects, thereby influencing the mechanical and for cleaning the LMFBR elements. Avoid vigorous cleaning
chemical properties. If the temperature of the fuel element agents, such as acids or strong bases, unless these agents are
becomes excessive because of decay heat, then provide ad- the only means of effectively removing the surface deposits.
equate cooling. Ordinarily, this will be water or sodium for 5.1.4.3 If the composition of the crud or loosely adhering
light-water reactor (LWR) and liquid metal fast-breeder reactor surface deposits is to be determined, then remove the samples
(LMFBR) fuel rods, respectively. The coolant should not have by scraping the element with a suitable instrument. Take
any detrimental effect on the cladding. special care to avoid contamination of the sample with metallic
5.1.1 Handling: particles scraped from the element or the instrument.
5.1.1.1 Exercise utmost care in handling and packaging the
fuel element or fuel rod. Clean each item in such a manner as 6. Visual Examination
6.1 Place the element (for example, fuel rod, plate, etc.) to
be examined in a suitable holder. The holder should provide
10
Zircaloy is a registered trademark of Westinghouse Electric Corp. means of manipulating the element so that all areas of interest

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can be examined conveniently with a minimum of handling. bowing is not reflected in the length measurement, indicate so
6.1.1 The holder should be sufficiently rigid to minimize the in the data.
possibility of movement during photographing. 7.5 Diameter Measurements:
6.1.2 An appropriate scale should be incorporated into 7.5.1 It is important that the surface of the element being
either the holder or the viewing instrument to aid the observer measured be clean. Document the cleanliness of the surface of
in establishing relative scale and magnification and to provide the element. In a manner least destructive to the element
a convenient method of locating specific areas with reference cladding, wipe away loose extraneous material (for example,
to a fixed point, such as the end of a fuel rod. Use a color particulates) adhering to the surface.
standard if color photography is utilized. 7.5.2 Take the measurements performed with a micrometer
6.2 Perform visual examinations either in a hot-cell facility or similar device at two or more positions at each measurement
or in an underwater facility, such as a spent-fuel pit. Use location. Take these measurements at equally spaced positions,
viewing instruments, such as periscopes, telescopes, remote if possible, around the circumference of the rod. Use minimum
stereomicroscopes, or closed-circuit television systems. or known force devices when measuring readily deformed
6.2.1 The instrument should be equipped with interchange- shapes such as thin-wall fuel elements. Centering is an impor-
able eyepieces, interchangeable or variable focal length (zoom) tant consideration.
objectives, or some other convenient method for obtaining a 7.5.3 Select the axial location of diameter measurements on
range of magnifications. a fuel rod to characterize adequately the dimensional stability
6.2.2 Means should be provided for documenting the con- or performance of the rod. If possible, use the same location as
ditions and appearance of the cladding with photographs. This the preirradiation measurements.
is best accomplished with a camera attached to the viewing 7.5.4 It is preferable that continuous diameter measure-
instrument or by the use of video tape for television examina- ments be taken. This can be done by a profilometer, employing
tion. Give a written description of the visual examination one or more dial indicators, LVDTs, or other suitable sensing
features to augment the photographs or video tape. devices, that bear on the fuel rod. Means can be provided to
7. Dimensional Measurements advance the sensing head axially as the rod is rotated and to
record the output of the sensing head, thereby obtaining a
7.1 Calibration: continuous trace of the fuel rod surface. This will reveal not
7.1.1 Calibrate all measuring apparatus by checking its only gross changes in diameter, but other anomalies such as
indicated readout against standards. ridging, blisters, ovality, etc.
7.1.2 Certify any standards, gage blocks, etc., used, and it is 7.6 Thickness Measurements:
best if these standards can be compared directly to National
7.6.1 It is important that the surfaces of the element being
Bureau of Standards masters. If this is not possible, compare
measured be clean.
the standards to primary standards or masters.
7.6.2 Determine the thickness of noncylindrical fuel ele-
7.1.3 Include the dimensions of the standard, the applicable
ments (flat plates, convolutions, etc.) by using a micrometer or
limits of precision and accuracy, and the temperature at which
other suitable measuring device.
the measurements were taken in the certification report.
7.2 Surface Preparation—It may be necessary or desirable
8. Determination of Breach and Defect Location
to remove any loosely adhering deposits on the cladding
surface, so that the dimensional measurements are as accurate 8.1 Leak Tests—Experience has shown that defects in fuel
as possible. Tightly adherent oxide films can also affect the cladding cannot always be detected through a visual inspection
dimensional measurements. Therefore, use a metallurgical or dimensional measurements, or both. To detect defects
examination to determine exactly how these films affect the resulting in a breach of the cladding, some type of leak test is
dimensional measurements. frequently performed as follows:
7.2.1 Perform the removal of these loose deposits by me- 8.1.1 In the liquid nitrogen-methanol leak test, immerse the
chanical means, such as light brushing in demineralized water. item to be tested in liquid nitrogen for approximately 15 min.
7.2.2 Do not attempt to use vigorous chemical reagents to Then remove and quickly plunge the item into methanol. A
remove any of the tightly adhering oxide film which is leak is indicated by the presence of a steady stream of bubbles.
frequently present. To do so would risk removal of the Do not use this test if there is any reason to believe that the
corrosion films and base metal, thereby decreasing the value of cladding or fuel may be adversely affected by the thermal
dimensional measurements and the corrosion data obtained shock involved or that it might undergo a phase transformation.
from the film thickness measurements. 8.1.1.1 In principle, the liquid nitrogen penetrates the clad-
7.3 Temperature Determination—In making any dimen- ding through a defect, such as a crack, pinhole, etc. When the
sional measurements, also measure the temperature of the rod is plunged into the warm methanol, the nitrogen immedi-
cladding. Due to gamma heating, the cladding surface tempera- ately vaporizes and escapes through the defect.
ture may be significantly higher than the ambient temperature 8.1.1.2 In the case of large leaks, all of the gas may escape
of the environment. from the rod in a short burst of bubbles. However, this type of
7.4 Length Measurements: leak or defect is ordinarily detected during the visual exami-
7.4.1 It is important that the ends of the element to be nation.
measured be clean and free of any deformation. 8.1.1.3 In the event of a very small leak, the bubbles may be
7.4.2 Adequately support the element to be measured. If so small or infrequent as to escape detection. Also, the defect

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may be actually covered or plugged with deposits of foreign the balance with traceable standards. Between measurements,
matter. return the balance to a zero or known value. As appropriate,
8.1.2 A helium leak test is generally more sensitive than the check the balance against working standard weights during the
liquid nitrogen-methanol. In addition, it has the advantage of measurement process.
being performed at room temperature, and thus does not 8.4.2.2 Periodically, replace or calibrate the working stan-
subject the cladding to thermal shock. This method can be used dard weights against certified reference weight standards.
to determine whether a leak is present but is not satisfactory for 8.4.3 Shield the fuel element being weighed from air
actually locating the defect. currents that could adversely affect the accuracy of the data
8.1.2.1 In this test, expose the rod to an external helium obtained.
pressure, remove from the pressurization chamber, then insert 8.4.4 Report the calibration data and measurement results
into the leak test chamber. Then evacuate the chamber and with the system accuracy stated. Suspect defective elements
measure the leak rate with a helium leak detector. can be identified as those in which the difference between the
8.1.2.2 Variations of this test make it possible to perform the preirradiation and postirradiation weights is significantly
test after the rod is punctured or sectioned. This test provides greater than the system accuracy for both measurement sys-
satisfactory results only when there are interconnecting voids tems.
throughout the length of the item to be tested. 8.5 Eddy-Current Cladding Integrity Testing—Eddy-current
8.2 Dye Penetrant Inspection—Various types of dye pen- nondestructive testing techniques provide a means of testing
etrant inspection may be used to detect surface flaws or cracks. the integrity of the cladding material of nuclear reactor fuel
Use Test Method E 165 as a guide. elements without contacting the cladding. By these techniques,
8.2.1 In general, clean the cladding surface to obtain con- it is possible to detect (1) the location of a breach in elements
clusive results. that have been identified as “leakers” by other test methods,
8.2.2 The presence of a tightly adhering oxide film can and (2) defect areas in cladding after irradiation, but prior to
render the results of a dye penetrant inspection inconclusive. breach.
8.3 Ultrasonic Inspection—Ultrasonic inspection provides a 8.5.1 Eddy-current testing does not require a liquid coupling
means to detect defects on the hidden, as well as exposed, medium. Therefore, the cladding is maintained free of contact.
surface of fuel cladding. It may also be applied to the Employ either an encircling coil that tests the entire element
measurement of cladding wall thickness and the nondestructive circumference in one pass or a probe coil that tests only a small
examination of welds, brazed joints, etc. (about 15 deg) segment of the clad circumference at a time.
8.3.1 Inasmuch as either water or a low-viscosity oil is The latter is somewhat more sensitive and provides easier
required to couple the transducer with the target, perform this interpretation of defect location with respect to circumferential
inspection in an underwater facility or in a tank of water in a orientation and inner or outer surface of the cladding.
hot cell. 8.5.2 The basic mechanical system requires a means of
8.3.2 The basic mechanical equipment generally required holding the test item and the sensing coil and providing the
for ultrasonic inspection includes suitable holding fixtures for appropriate relative motion between the two. Position the test
both the target and the transducer. item accurately with respect to the test probe or encircling coil
to maintain repeatable coupling.
8.3.2.1 The target-holding fixture must be capable of mov-
8.5.3 Basic electronic equipment includes the necessary
ing the target with respect to the transducer or the transducer
controls for operation of the mechanical equipment, eddy-
with respect to the target, or moving both, so that the entire
current signal generator and receiver, and display and record-
area of interest may be inspected (for example, if the target is
ing devices such as an oscilloscope and strip-chart recorder.
a fuel rod, a device for rotating the rod is required).
8.5.4 Interpretation of results depends on the use of cali-
8.3.2.2 The transducer-holding fixture must maintain the
brated and well characterized standards. Standards should
desired orientation of the transducer and the distance away
contain defects that approximate typical defects. They should
from the target.
possess several defect sizes located both on the inside surface
8.3.3 Basic electronic equipment should include an oscilla- and the outside surface. Standards should also contain typical
tor to produce the signal for the transducer, a pulsing circuit, a internal components, such as fuel pellets, spacers and springs,
receiver to detect the pulse echo, and a display or readout cladding variations, or components that would simulate these
device, such as a strip-chart recorder or an oscilloscope. items.
8.3.4 A calibrated standard is necessary to adjust the equip-
ment so that the size of a defect may be estimated. 9. Gamma Scanning
8.4 Weight Measurement: 9.1 Employ gamma scanning to determine the axial distri-
8.4.1 Employ weight measurement, particularly in sodium- bution of cladding activation and fission-product activity, to
bonded elements, to detect the presence of a breached fuel determine the position and dimensions of element components,
element by the indication of a greater-than-expected weight and to help determine suspect breached elements by loss of
change due to egress of sodium bond or ingress of primary fission-product activity.
coolant. 9.1.1 Use the distribution of the activation of the cladding or
8.4.2 The balance must possess sufficient sensitivity to specific fission-product activity to determine the relative fast
detect the expected weight change. and thermal fluence received by the various portions of the
8.4.2.1 Prior to any series of weight measurement, calibrate element.

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9.1.2 Determine the position and dimensions of element 11.2 Specimen Preparation:
internal components (fuel pellets, bond-sodium level, etc.) by 11.2.1 Obtain a section of the fuel rod or plate with the fuel
counting the appropriate specific activities. intact in a manner that prevents excessive heat generation or
9.1.3 Deficiency of fission-product activity within the gas cold working during sectioning. Mount this section in a
plenum or bond-sodium indicates a breach of cladding. A loss cold-setting compound that cures at temperature less than
of bond-sodium and dissolved fission products within the 150°C or lower and is resistant to gamma-irradiation and to
bond-sodium indicates breach below the sodium level. deterioration or swelling at temperatures as high as 150°C.
9.2 The elements to be gamma scanned are moved past a Maintain the record of specimen location and orientation,
thin slit through which the gamma and beta rays are allowed to particularly if the orientation of the rod with respect to the rest
pass. The gamma and beta rays are then collimated by a of the assembly is known.
shielded slit over a suitable distance. The collimated beam is
11.2.2 Rounding of the edges of the cladding during grind-
directed at a high-resolution detector attached to a monitor and
ing or polishing is undesirable, especially when evaluating the
readout system. The design of the system will depend on the
corrosion behavior. If routine polishing techniques are not
size, shape, and activity of the item being scanned. A multi-
channel analyzer can be employed to identify and measure the available to prevent this rounding of the surface, then prevent
activity produced by individual nuclides. the rounding by mounting the specimen in a potting compound
containing a fine abrasive material such as aluminum oxide or
10. Neutron Radiography plating the specimen with a metal such as nickel or chromium.
10.1 Neutron radiography is a nondestructive technique for The latter method is undesirable in cases where examination of
determining the internal condition of fuel elements or experi- the fuel within the cladding is to be performed.
mental capsules. A film image is produced, with the film 11.2.3 Prepare the metallographic specimen in accordance
density being a function of the neutron attenuation character- with Methods E 3. In some instances, it may be desirable to
istics of the material being radiographed. avoid grinding and polishing using an aqueous media. Certain
10.2 Neutron radiography provides information such as: organic liquids can be effectively used as a coolant in these
internal component location, fuel condition (pellet separations, instances. Take special care, however, to prevent heating of the
voids, fissile density variation, cracking, etc.), dimension of specimen during grinding. The final polishing steps will vary
components, water ingress, bond-sodium level, hydride forma- with the material being processed and should be established on
tion in cladding, etc. a trial specimen prior to conducting the examination.
10.3 Place the fuel elements including length and contrast 11.2.4 After the specimen is polished satisfactorily, examine
standards in a collimated thermal neutron beam emanating the specimen in the as-polished condition. If microprobe
from the neutron source (which may be a reactor, accelerator, analysis is to be performed, then complete it before etching.
radioisotope, or other source of neutrons). Place a neutron Following this examination, etch the cladding or fuel to
detector, usually a dysprosium or indium foil, behind the fuel establish the desired microstructural characteristics. It is pref-
elements and expose to the neutron beam. Indium resonance erable to examine the fuel first since the etchants used for the
energy neutrons (1.4 eV) provide more penetration of nuclear cladding may attack the fuel thereby destroying areas of
fuels and are therefore useful in revealing internal character- interest. In many instances, the corrosion rates are enhanced by
istics in the fuel. With this technique, place a thermal neutron irradiation. Therefore, take special care to avoid overetching.
attenuater (gadolinium, cadmium) in front of the indium The etchants used for cladding are generally somewhat differ-
neutron detector. Subsequently place the detector in contact ent than those for fuels. In the examination of both materials it
with X-ray films and allow to decay for three or more half-lives is usually necessary to repolish and reetch the specimens after
to produce the image. Since the radiation emanating from the one examination has been completed.
activated neutron detector foils is low-energy, it is very 11.3 Fuel Cladding Interaction:
important to ensure that the foil and films are in intimate
contact and that no foreign material is allowed between the foil 11.3.1 Fuel-cladding contact, especially at high tempera-
and film. Failure to do so will result in poor-quality radio- tures and high burnups, can lead to both chemical and
graphs. The film thus exposed can then be processed by using mechanical interaction. The extent of both the chemical and
normal X-ray film processing techniques (see Guide E 94 as a mechanical interaction is often quite important in establishing
guide). Dysprosium foils provide more detail in non-fuel the useful life of the fuel element. The mechanical interaction
components of a fuel element and are used in generally the is the result of differential thermal expansion between the fuel
same way as for indium foils. and cladding. The chemical reaction can either be a reaction
between the cladding and the fuel or a reaction between the
11. Metallography fission products and the cladding.
11.1 Significance—The cladding should be examined met- 11.3.2 Determine the depth of attack and the cause of the
allographically to determine the extent of any microstructural attack. Knowing the depth of the attack is very important,
changes and the corrosion behavior resulting from the exposure especially when sections of the cladding are to be used for
in the reactor. The optical microscope can provide a significant determining the mechanical properties. Make special efforts to
amount of data regarding the in-reactor behavior. The electron preserve this interaction. This may be difficult as these reaction
microscope may enhance the accuracy of the analyses and products are often destroyed during normal handling and
interpretation. mounting operations. Impregnation of the specimens with

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cold-setting epoxy compounds prior to any major metallo- effects of operation on the microstructural changes in the
graphic preparations is useful for preserving the as-irradiated cladding.
conditions. The epoxy resin, however, has a tendency to 11.5.2 The cladding on many fuel elements is often less than
destroy the chemical nature of some of the fission products. 0.38 mm in thickness. Furthermore, the hardness may vary
The mode of attack (for example, stress-corrosion cracking, through the cladding thickness. Many hardness tests are
intergranular attack or cracking and general uniform corrosion) therefore not suitable for this material. The Knoop and Vickers
should also be established. test have generally been found suitable for determining the
11.3.3 Measure the width of the fuel-cladding interaction hardness of the cladding. Therefore, follow the procedure in
zone from a specified plane of polish with a metallograph accordance with Test Method E 92. Take special care to ensure
containing a calibrated filar eyepiece or from a photograph of that valid results are obtained.
calibrated magnification. 11.5.3 Obtain at least five individual readings at each
11.3.4 From the as-polished surface, obtain the composition location. Obtain hardness at a minimum of three locations:
and composition gradients by scanning the sample surface with inside surface, outside surface, and mid-radius. If possible,
ion or electron microprobes and performing electron or mass determine the hardness at areas of abnormal appearance.
spectroscopy.
12. Density Measurement
11.4 Corrosion Behavior:
11.4.1 Certain metals form an adherent protective film 12.1 Scope—This method covers the determination of the
during corrosion, whereas other metals corrode by the loss of density of cladding using immersion techniques. Accuracies of
material. In the former case, it is possible to measure the oxide 0.05 % can be achieved using this method. However, the
film thickness and to convert the oxide film thickness to a mass obtained accuracy will vary with the mass of the specimen.
gain and to determine whether corrosion produces any com- Methods and definitions of terms for density measurement of
positional changes through the thickness of the cladding. In the solids by immersion techniques are documented in Test
latter case, it is not possible to establish the corrosion rate Method F 77 and Terminology E 12. The calculation of the
unless the mass of the specimen is known prior to exposure to density of solids to make determinations to better than 0.05 %
the corrosive environment. However, it is possible to determine requires careful attention to technique. Many factors, such as
whether corrosion occurs by pitting, intergranular attack, etc., air buoyancy, temperature differences, surface tension of the
or produces compositional variation within the metal. liquid, chemical changes, and calibration of the density of the
11.4.2 Oxide Film Thickness—The oxide film on many displacement liquid, contribute significantly to the results.
alloys, in particular zirconium alloys, is very seldom com- 12.2 Definition:
pletely uniform in thickness. Consequently, a large number of 12.2.1 density—the mass per unit volume, expressed in
measurements must be made to obtain a reliable value for the grams per cubic centimetre.
film thickness. Before making the measurements, examine the 12.3 Apparatus:
entire periphery of the as-polished cladding to determine 12.3.1 Chemical Balance, capable of measuring to 0.1 mg.
whether there are any areas of abnormally thick or thin 12.3.2 Thermometer or Thermal Sensor, capable of being
corrosion films. If such areas are present, treat these areas in an read to 0.2°C within the range from 15 to 25°C.
individual manner. If no abnormally thick or thin areas are 12.3.3 Hook and Wire—A hook suspended by a wire about
observed, then take at least eight film thickness measurements 0.13 mm in diameter or less if possible, both materials being
at equally spaced locations around the periphery. Take these fabricated from corrosion-resistant material. This arrangement
measurements with a filar eyepiece with an accuracy of 6 0.1 can be used either to support the specimen or a wire mesh
µm. The resulting film thickness, Tf, can be converted to a mass basket that contains the specimen.
gain, M, using the following equation: 12.3.4 Wire Mesh Basket, constructed from a corrosion-
resistant material to suspend the specimen during immersion
M 5 Tf 3 K (1)
when the hook and wire combination is not a feasible method
K will vary from material to material, and this value must be of suspension.
determined experimentally. For Zircaloy-2 and Zircaloy-4,t K 12.3.5 Tank, with a sufficiently large opening to allow
is equal to 15.6 mg/dm2·µm. unhindered introduction and removal of the specimen and
11.4.3 Hydrogen Content—Evaluate the orientation of the specimen holder to and from the immersing liquid. For small
hydride platelets within Zircaloyt fuel cladding using metal- specimens, water currents and motion caused by introducing
lographic techniques. Determine the hydrogen content using the specimen into the bath must be eliminated before weighing
the vacuum extraction techniques in accordance with Methods proceeds. If possible, a constant temperature liquid container
E 146. Because cooling rates and thermal gradients can affect should be used.
the size and concentration of hydride platelets, quantitative 12.4 Materials:
metallographic techniques for determining hydrogen content 12.4.1 Test Liquid or Immersing Fluid—Some acceptable
are not recommended. common fluids used for density measurements are as follows:
11.5 Hardness: 12.4.1.1 Distilled water containing a wetting agent such as a
11.5.1 Irradiation of the fuel elements can produce gross or detergent,
localized changes in the hardness of the cladding. The hardness 12.4.1.2 Carbon tetrachloride, CCl4,
of the irradiated cladding can provide some indication of the 12.4.1.3 Bromobenzene, C6H5Br, and
strength of the cladding and possibly some insight into the 12.4.1.4 Perfluorotributylamine, (C4F9)3N.

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12.5 Procedure: 13.2.1 Hot Vacuum-Extraction—Hot vacuum-extraction
12.5.1 Weigh the test specimen in air. techniques are methods used to remove absorbed and dissolved
12.5.2 Immerse the specimen and holder into fluid. Allow gases from solids. The usual manner by which this is accom-
sufficient time for the temperature of the specimen and the plished is to heat the solid in a vacuum at a sufficiently high
temperature of the bath to equilibrate. Ten minutes is generally temperature to allow removal of the gases from the solid by
sufficient for samples of 10 g or less. Measure and record the diffusion and collect the released gas. The gas can then be
temperature of the fluid to 0.2°C. analyzed by accepted standard methods for gas analysis. The
12.5.3 Determine the density of the immersing fluid. This techniques and methods used for this determination on irradi-
determination can be made either by weighing a known volume ated samples are identical with those used for unirradiated
of fluid or by determining its buoyancy on a precision- samples with the exception of the special handling required to
machined standard specimen such as Invar or gold. protect personnel from the residual radioactivity of the speci-
12.6 Calculation: men. For hydrogen analysis by this technique, see Methods
12.6.1 Density of Liquid—Obtain the density of the liquid E 146.
as specified in 12.5.3. Since the density of most liquids varies 13.2.2 Vacuum Fusion—Vacuum fusion analysis is a tech-
with temperature, it will be necessary to make a correction if nique by which gas, adsorbed, absorbed, and combined in a
the specimen and liquid densities were measured at different solid, is released by melting or fusion, and the gas is collected
temperatures. for subsequent analysis. The methods recommended for irra-
12.6.2 Density of Specimen—Calculate the density of the diated materials are similar in most respects to those for
specimen as follows: unirradiated materials, with the exception of the special tech-
D 5 $~WA 3 d! 2 ~WL 3 D!%/~WA 2 WL! (2) niques required to protect personnel from the residual radio-
activity and contamination of equipment with radioactive
where: materials. The techniques vary slightly with each subject
D = density of specimen at temperature T, g/cm3,
material and recommended procedures are not currently avail-
WA = mass of specimen in air, g,
WL = mass of specimen in liquid, g, able.
d = density of liquid at temperature T, g/cm3, and 13.2.3 Microprobe:
D = density of air, g/cm3. 13.2.3.1 Scope—The term “microprobe analysis” covers a
12.6.3 Temperature Corrections—Temperature can cause number of operations ranging from quantitative chemical
perturbations in the equation in 12.6.2. The equation can be analysis to qualitative photographic displays. There are several
modified to include variations in temperature as follows: ways in which the electron microprobe can be used depending
D 5 $~WA 3 d3 X! 2 ~WL 3 D 3 Y!%/~WA 2 WL! (3) on the application of the data to be obtained. These include:
X 5 1 2 K~T 2 TL! (1) X-Ray Spectrum Scan—A method to determine the
elements present in an unknown sample.
Y 5 1 2 K~T 2 TA!
(2) Line Scan—A semiquantitative method of determining
where: the relative concentration of an element across a portion of the
K = volumetric coefficient of thermal expansion, sample.
and (3) Step Scan—A line scan in which the specimen is moved
T, TL, TA = temperature of interest, of the immersion liq- through the electron beam in finite increments, and X-ray
uid and of the air, respectively. counts are recorded during these incremental steps.
When TL = TA, X = Y and the equation reduces to a
(4) Area Scan—The X-ray spectrometric method set to
correction involving K and the temperature of
receive the characteristic X-ray wavelength from a specific
interest.
element that can be used to scan a given area.
12.7 Report—The report shall include the following:
12.7.1 Chemical composition of specimen, 13.2.3.2 Procedure—Prepare the sample in the same man-
12.7.2 Previous mechanical and thermal treatment, ner as a metallographic specimen. Obtain sufficiently smooth
12.7.3 Irradiation data, including reactor, irradiation tem- surface for examination by a final polish with 0.25-µm dia-
perature, total fluence, neutron dosimetry and monitor, and mond paste. A light chemical or electrolytic etch may be
instantaneous flux, required after polishing to bring out the metallurgical structure
12.7.4 Mass of specimen, of the surface. Examine test samples in the as-polished
12.7.5 Density of specimen to three significant figures, condition if there is danger of removing elements of interest by
12.7.6 Temperature at which density measurements are etching. The procedures for examination are highly dependent
made, and upon the type of examination required. The examinations
12.7.7 Immersion liquid. generally can be classified into two types, qualitative analysis
and quantitative analysis as follows:
13. Analytical Methods (1) Qualitative Analysis—When only some indication of
13.1 Routine—Routine analytical methods are covered in the elements in the subject material is known and positive
the Annual Book of ASTM Standards, Section 3, where over identification is desired, use the following techniques: (a)
100 standard methods are described. spectrum analysis for the unknown elements; (b) area scan to
13.2 Special: show the distribution of the elements present; and (c) line scan

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to show the change in compositional distribution of the (3) longitudinal specimens obtained from a segment of tubing,
elements present. and (4) short rings obtained from the tubing. Where possible,
(2) Quantitative Analysis—Use the following techniques the type of specimen employed shall conform to the require-
when the compositional elements of the sample are known but ments of Test Methods E 8. In some instances, it may not be
their relative amounts are unknown: (a) single spot analysis possible to select a specimen that conforms to Test Methods
and (b) trace analysis over a small zone. E 8 because of the configuration of the cladding or because of
13.2.3.3 Report—Standardization of report forms is not the limited irradiation space. Where it is not possible to use
applicable for reporting microprobe analysis because of the standard test specimens, it is recommended that the length to
lengthy remarks that often are needed to accompany the data. width ratio of the gage length be about 4.0. The thickness of the
specimen should be equal to that of the cladding, and nonirra-
14. Mechanical Property Test diated specimens shall be of the same size and shape. Make
14.1 Selection of Materials—Obtain the chemical composi- every effort to establish the correlation between the type of
tion, properties, and metallurgical structure of the material specimen used and a standard specimen. Attach the grips,
before irradiation for all materials used to determine the extender tab, or tubing fittings in such a way to avoid bending,
mechanical properties. This information should include the cutting, or changing the material properties near the attach-
following: ment. Perform the tension test at temperatures and strain rates
14.1.1 Processing history, including such information as most closely simulating service condition or expected condi-
metal designation, manufacturer, heat number, fabricating tions.
procedures, and heat treatment. (When possible, archive 14.3.2 Burst Specimens—Two types of specimen designs
samples shall be maintained and stored for future reference.), will be generally utilized: (1) a piece of tubing cut from a
14.1.2 Chemical composition, reactor cladding section that contained a fuel material, and (2)
14.1.3 Original location and orientation of all test speci- a specimen designed and irradiated as a study material. Each of
mens in the parent material, these specimens will vary slightly because of its history. The
14.1.4 Appropriate mechanical properties prior to radiation, cladding will generally be open at each end and can be closed
determined on specimens taken from a location and orientation by welding or by mechanically attaching plugs in one end. The
equivalent to that of the irradiated specimens, second specimen may be open or have an end plug welded in
14.1.5 Optical micrographs showing the structure of the place prior to irradiation. In all cases, the basic specimen will
material at the test location and, if possible, electron micro- consist of a section of tubing closed at one end by a blind plug
graphs, and open at the other end to allow pressurization. Irradiated
14.1.6 Average grain size of these materials, estimated in and nonirradiated control specimens shall be of the same size
accordance with Test Methods E 112, and for steels, the and type. The ratio of gage length to diameter (L/D) should be
inclusion content shall be determined in accordance with Test >10; however, where shorter specimens are used to conserve
Methods E 45, material or reactor space, run adequate testing to ensure the
14.1.7 Other information such as hardness, the variation in absence of end effects that alter the test information.
hardness, and other mechanical properties with locations and
14.3.3 Creep Specimens:
orientations through the thickness of the material, etc.,
14.1.8 Crystallographic orientation of the as-fabricated ma- 14.3.3.1 Test specimens of the type, size, and shape de-
terial, and scribed in Test Methods E 8 are generally suitable for tests at
14.1.9 Density of the material being irradiated. elevated temperatures. Where it is not possible to use standard
14.2 Removal of Fuel: test specimens, irradiated and nonirradiated specimens shall be
14.2.1 For many of the mechanical property tests, it will be of the same size and shape, and every effort shall be made to
necessary to remove the fuel from the cladding. Where the establish the correlation between the type of specimen used and
mechanical and chemical interaction between the fuel and a standard specimen. When the dimensions of the material
cladding has been minimal, removal of the fuel should not be permit, except for sheet and strip, the specimens should have
a problem. Where the fuel-clad interaction has been large, then circular cross section over the gage length. The ratio of gage
special techniques must be developed to remove the fuel as length to diameter should be 4. If different ratios are used,
there are no standard techniques available. direct specific attention to this fact in reporting the test results.
14.2.2 Both chemical (dissolution of the fuel) and mechani- The reduced section of sheet specimens do not need to be
cal (grinding or drilling of the fuel) techniques have been used longer than 57 mm or wider than 25 mm. Take sheet specimens
to remove the fuel. Regardless of the technique used, take from the sheet stock in the direction of rolling, unless other-
special care to prevent damage of the cladding. Evaluate any wise specified.
procedure that is developed on some dummy specimens before 14.3.3.2 Specimens of circular cross section may have
being used. Then evaluate the dummy specimens to ensure that either threaded or shouldered ends for gripping.
the mechanical or chemical attack has not affected the proper- 14.3.3.3 For sheet or strip specimens, some modification of
ties of the cladding. the standard specimens described in Test Methods E 8 is
14.3 Design of Specimens: usually necessary to permit application of the load to the
14.3.1 Tension Specimens—In general, four types of speci- specimen in a furnace. If the material available is sufficient, the
mens can be obtained from the various types of fuel cladding: use of elongated shoulder ends to permit gripping outside the
(1) full-size tubular sections, (2) specimens from sheet or strip, furnace is the easiest method. When the length of the specimen

8
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is restricted necessarily, several methods of gripping are used, plug welded in place prior to irradiation. In all cases, the basic
as follows: specimen will consist of a section of tubing closed at one end
(1) High-temperature sheet grips similar to those illustrated by a blind plug and open at the other end to allow pressuriza-
in Test Methods E 8 and described as self-adjusting grips. tion. Irradiated and nonirradiated control specimens shall be of
These have been proved satisfactory for testing sheet materials the same size and type. The ratio of gage length to diameter
that cannot be tested satisfactorily in the usual type of wedge should be >10; however, where shorter specimens are used to
grips, conserve material or reactor space, run adequate testing to
(2) By means of extension tabs welded or brazed to the ensure the absence of end effects that alter the test information.
specimen shoulders and extending to grips outside of the Insert a quartz or fused silica rod into the specimen before
furnace, or attaching the end caps. The quartz rod should allow for gas
(3) Specially designed grips that conform to and apply the flow from one end of the specimen to the other. The quartz rod
load against the fillets at the end of the gage length. minimizes the gas volume (that is, stored energy), thereby
14.3.3.4 Test full sections of tubing using modified tubing producing a burst event typical of a fuel pin.
fittings as grips or as closures when using the tubing as a 14.4 Preparation of Specimens:
biaxial test specimen in creep. 14.4.1 Tension Specimens:
14.3.4 Tubular Creep Specimens: 14.4.1.1 Test specimens should be of uniform thickness
14.3.4.1 A variety of creep tests using tubular specimens are throughout the gage length.
possible depending on the methods for applying the load and 14.4.1.2 Obtain the specimens from the cladding using any
the results desired. These tests include uniaxial creep, biaxial suitable machining technique that minimizes the amount of
creep using an internal pressure, and biaxial creep using cold work introduced into the specimen. Cool the specimens
internal pressure and axial tensile or compressive loads. The with a suitable medium where heat may be generated during
type of information required will determine which test to use. machining.
Tests to compare different materials can generally use the 14.4.1.3 All surfaces, both machined and unmachined, of
uniaxial test or biaxial creep test using internal pressurization. the finished specimen shall be smooth and reasonably free of
Creep tests to obtain precision data for code development will undercuts and scratches. Do not use chemical methods for
generally require the use of biaxial creep specimens using a polishing or deburring, because the chemical could selectively
combination of internal pressure and axial loads. attack the specimen and result in poor specimens.
14.3.4.2 The internal pressurization tests can use a short 14.4.2 Burst Specimens:
section of tubing, L/D ratio of >10, especially if the test is run 14.4.2.1 Test specimens should be of uniform wall thickness
similar to standard burst test. throughout the gage length.
14.3.5 Fatigue Specimens—Test specimen design depends 14.4.2.2 Keep the type of end closure constant. Several
on the type of testing machine used and the type of fatigue to types of closures have been found to be successful. Utilize a
be simulated. Configurations for specimen gage lengths suit- type that will produce an effective closure and not contribute to
able for testing in stress-controlled high-cycle fatigue (greater or detract from the properties of the tube. Common closures
than 50 000 cycles) are provided in Practice E 466. Configu- include end plugs welded in place, mandrels held in place by
rations for specimens suitable for testing in strain-controlled, pressure fittings, and blind-end pressure fittings. Attach a
low-cycle fatigue are provided in Practice E 606. Both irradi- pressure fitting for introduction of the pressurization fluid or
ated and nonirradiated controls shall be of the same size and gas to the open end. Take care to ensure that the attachment of
shape. pressurization fittings does not affect the properties of the
14.3.6 Bend Specimens—Specimen design for bend tests is tubes. Where welded end plugs are used, constrain the cladding
relatively fixed. The recommended specimen is 130 mm long adjacent to the weldment so that failure does not occur in the
with a width-to-thickness ratio of 20:1 for thicknesses of 1.3 to heat-affected zone. Where applicable, use the procedures
2.5 mm. Specimens thinner than 1.3 mm shall be a minimum recommended in Specification B 353 as a guide.
of 25.4 mm wide. The maximum recommended thickness is 14.4.3 Creep Specimens:
2.5 mm. When it is not possible to use the standard 130-mm 14.4.3.1 Test specimens should be of uniform cross section
long specimen, irradiated and nonirradiated specimens shall be throughout the gage length and should be within the following
of the same size, and every effort shall be made to establish the limits:
correlation between the subsized specimen and a standard Nominal Diameter or Tolerance, Percent of Di-
Width, mm ameter of Width
specimen. The same specimen design is applicable for both 2.5 60.5
room temperature and elevated temperature testing. 6.5 60.4
14.3.7 Transient Specimens—Two types of specimen de- 8.0 60.3
13.0 60.2
signs will be generally utilized: (1) a piece of tubing cut from
a reactor cladding section which contained a fuel material and The diameter or width at the ends of the reduced section
(2) a specimen designed and irradiated as a study material. should not be less than the diameter or width at the center of
Each of the above specimens will vary slightly because of its the reduced section. It may be desirable to have the diameter or
history. The cladding will generally be open at each end and width of the reduced section of the specimen slightly smaller at
can be closed by welding or by mechanically attaching plugs in the center than at the ends. This difference should not exceed
one end. The second specimen may be open or have an end the tolerance limits specified above.

9
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14.4.3.2 All surfaces, both machined and unmachined, of the finished specimens must be as smooth as possible and free
the finished specimens shall be smooth and reasonably free of of undercuts and scratches. Undercuts and scratches will
undercuts and scratches. Exercise special care to minimize the reduce the endurance limit of most materials. Exercise special
disturbance of surface layers by cold work. Exercise great care care to minimize disturbance of the surface layers by cold
to minimize eccentricity in the specimen to provide for axial work. Regardless of the machining, grinding, or polishing
application of the load. When extension tabs are used for sheet method used, remove the final metal in a direction approxi-
or strip samples, perform the brazing or welding in a jig or mately parallel to the long axis of the specimen.
fixture to ensure accurate alignment, and take precautions to 14.4.6 Bend Specimens:
avoid overheating the specimens. Where loading pins are used 14.4.6.1 Test specimens should be of uniform cross section
for sheet or strip specimens, accurately center the pin holes on throughout their length, width, and thickness. The maximum
extensions of the center line of the gage sections. allowable limits are 6 0.01 mm in the gage-section area of the
14.4.3.3 Overall specimen length, length of shoulders,
sample.
threaded ends, etc., should not be less than prescribed in Test
Methods E 8, or by customary sheet practice for specimens for 14.4.6.2 All surfaces, both machined and unmachined, of
tension tests. Increasing the length of the shoulder facilitates the finished specimens should be smooth and reasonably free
obtaining the proper temperature distribution and axiality of of undercuts and scratches. Exercise special care to minimize
loading. disturbance of surface layers by cold work.
14.4.4 Tubular Creep Specimens: 14.4.7 Transient Test—See 14.4.2.1 and 14.4.2.2.
14.4.4.1 Select sections of cladding that have minimum 14.5 Procedure:
variations in wall thickness, ovality, and eccentricity. Decrud 14.5.1 Tension Test:
the irradiated fuel cladding and remove the fuel. Make every 14.5.1.1 Conduct the tension test in accordance with Test
effort to avoid damage of the cladding during removal of the Methods E 8 or E 21, except for the following modifications:
fuel. Specimens requiring application of an axial load should
(1) Measure and control the strain rate, when possible, by
be long enough to minimize the end effects of the grips.
Specimens having a gage length of 70 to 100 mm should be at using a suitable extensometer attached to the gage length or the
least 400 mm long. This will depend on the type of grips and shoulders of the specimen. Rate of crosshead separation is a
the length of the furnace. permissible method of controlling the speed of testing; when
14.4.4.2 The specimen for axial creep tests requires no speed of testing is controlled in this manner, determine the
special preparation as a section of the tubing will be adequate. accuracy of this method.
Take special care in the design of the grips to ensure that (2) If the test is interrupted for removal of the extensom-
slippage does not occur and that they do not fracture the eter, make every effort to ensure that the load does not decrease
cladding embrittled by irradiation. significantly during the test.
14.4.4.3 The biaxial creep tests will require special end (3) Record the complete stress-strain or load-deflection
fittings, one end being capable of introducing the gas pressure. curves.
The optimum design is a special end cap welded to the tubular (4) Determine the uniform elongation, which is the in-
specimens. The end cap can be designed such that grips may be crease in length of the gage length prior to the onset of necking,
used to apply the axial load. Swagelockt11 devices can also be expressed as a percentage of the original gage length, from the
modified to be acceptable as end caps. These devices, however, elongation recorded by the extensometer at the maximum load.
are not as satisfactory as the welded end plugs for high- The uniform elongation can often be determined from the
temperature and long-duration tests. change in cross-sectional area of the unnecked portion of the
14.4.5 Fatigue Specimens: broken tension test specimen.
14.4.5.1 Test specimens should be of uniform cross section 14.5.2 Burst Test:
throughout the nominal gage length and within the following
14.5.2.1 Conduct the temperature control in accordance
limits:
with Practice E 139 and using Specification B 353 as a guide.
Nominal Diameter or Tolerance, Percent of Di-
Width, mm ameter or Width 14.5.2.2 Apply the pressure to the tube at a controlled,
2.54 60.5 constant, or known rate. Apply this pressure with oil, water,
6.35 60.4
8.13 60.3
gas, etc., dependent upon the test temperature and the type of
12.83 60.2 pressurization equipment. Avoid the use of equipment that
causes a pulsating pressure. The pressurization fluid should not
The diameter or width at the ends of the reduced section
cool the test specimen. Preheating of the fluid may be needed.
should not be less than the diameter or width at the center of
Consider instrumentating the test and pressurizing in a con-
the reduced section. It may be desirable to have the diameter or
trolled volume (strain rate) mode for better comparison and
width of the reduced section of the specimen slightly smaller at
possibly correlation with conventional tension tests.
the center than at the ends. This difference should not exceed
the tolerance limits specified above. 14.5.2.3 Do not apply the load until the specimen is uni-
14.4.5.2 All surfaces, both machined and unmachined, of formly heated and the thermal equilibrium is sufficiently
established to ensure that the temperature can be maintained
within the specified limits. Record a pressure versus strain
11
Swagelock is a registered trademark of Crawford Fitting Co. curve where possible.

10
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14.5.2.4 Obtain stress-strain data using the thick-walled- Experience indicates that specimens can be brought to a
tube relationship for an unrestrained, uniformly, internally temperature and the temperature stabilized adequately if suffi-
pressurized cylinder: cient attention is given to temperature adjustments prior to and
s 5 P ~RI 2 1 RO 2!/~RO 2 2 RI 2! (4)
subsequent to applying the load. Short preheat times require
special attention to temperature variables prior to and after
where: loading the specimen. It has long been recognized that a
s = hoop stress, Pa, practice of heating the specimens to within 28°C of the
P = internal pressure, Pa, temperature in 2 to 4 h with a final adjustment period of 20 h
RO = outside radius of the tube, mm, and results in good temperature stabilization. This practice is
RI = inside radius of the tube, mm. preferred when such prolonged heating periods do not intro-
This equation is applicable even when RO$ 1.05 RI. duce structural changes that affect the properties of the material
14.5.3 Creep Test: being tested or constitute poor utilization of equipment time.
14.5.3.1 Conduct temperature control and measurement in Note the practice that is used in the report.
accordance with Practice E 139 except for the following 14.5.3.5 Apply the load in such a manner as to avoid shock
modifications: loads or overloading due to inertia. Apply the load in incre-
(1) Temperature variation of the specimen from the indi- ments with strain readings between increments to provide
cated nominal test temperature shall not exceed 6 3°C for the stress-strain data for the application of the load. Apply the load
duration of the test. as quickly as possible within these limitations. Strain measure-
(2) Measure indicated temperatures prior to adjustments at ments for creep tests should measure all of the creep after the
least twice every working day. load is applied and, preferably, should measure the strain from
(3) Continuously record the indicated test temperature by a applying the load.
suitable device during the test. 14.5.3.6 For rupture tests, provide a suitable means for
(4) Indicated temperature variations along the gage length measuring the elapsed time between the complete application
of the specimen should not exceed the following limits: of the load and the time at which the fracture of the specimen
Up to 540°C, incl 62°C occurs to within 1 % of the elapsed time.
540 to 1090°C, incl 63°C
Over 1090°C 64°C 14.5.3.7 If any temperature disturbances cause the tempera-
ture of the specimen to rise above or below the limits specified,
(5) Overheating prior to attaining the limits specified shall
reject the test and retest. Exception may be made to this when
not exceed 1 % above the indicated nominal test temperature;
the length of time below the nominal temperature is so short
the duration of such heating not to exceed 10 min.
that it does not significantly influence the creep rate or rupture
(6) The control of bending moment during the testing of
time. Allowing the temperature to fall below the nominal
irradiated material is an important consideration. It is recog-
temperature reduces creep rate and prolongs rupture time, both
nized there is difficulty in obtaining the required alignment
characteristics being very sensitive to test temperatures. Low
standard specified in Practice E 139; however, make a con-
temperatures usually do not damage the material as do higher
certed effort to keep the bending moment as low as possible for
temperatures, which may accelerate the creep considerably.
postirradiation testing. When possible, obtain and report the
Consequently, under-temperatures should be cause for rejec-
alignment characteristics of the creep unit being used.
tion only when the time at that temperature significantly alters
14.5.3.2 The desirability of attaching the strain-measuring
the test results.
equipment to the specimen is clearly recognized; however, this
is not always possible because of the difficulties sometimes 14.5.4 Tubular Creep Test:
encountered due to the use of manipulators. Under carefully 14.5.4.1 All of the test procedures described in 14.5.3 are
controlled conditions, make strain measurements by measuring applicable to the tubular creep tests. The following additional
the movement in the load train. When this method is used, take guidelines are provided:
the following precautions: (1) make strain measurements on (1) Load Application—The biaxial strain in the tubular
control specimens by placing a suitable strain device on the specimens is generated by the internal gas pressure. Inert gases,
gage section of the specimen and on the load train, (2) then argon or helium, should be used to minimize reaction of the gas
make a correlation between the actual strain and the apparent and the cladding. A bottled gas with a precision pressure gage
strain, and (3) test a sufficient control specimen to establish this and regulator is satisfactory. The pressure gage should have an
correlation at each test temperature and for each method. accuracy of 6 35 MPa. Apply the axial load using a constant
14.5.3.3 Place the specimen in the test equipment and bring load-lever-arm creep machine or a standard tensile test ma-
to uniform temperature, taking care not to overheat the chine. In either case, the machine should be equipped with an
specimen beyond the nominal temperature. automatic beam-leveling device.
14.5.3.4 Do not apply the load until the specimen is uni- (2) Strain Meassurement—The strain can be measured in a
formly heated and thermal equilibrium is sufficiently estab- number of ways, depending on the information needed and the
lished to ensure that the temperature can be maintained within accuracy desired. Use micrometers and profilometers to mea-
the specified limits. Preheat for not less than 1 h after obtaining sure the diametral strain where accuracy isn’t too important
equilibrium temperature. The most important feature govern- and where total plastic strain is desired. These devices are used
ing the preheat time before applying the load to the specimen during post-test measurements and can only obtain data on
is the attainment of adequate control of the temperature. total plastic strain. Measure axial strain with micrometers or by

11
 E 453
measuring the distance between fiducial marks. The axial strain in strain of outer fibers. The stress calculated in the outer fibers
(plastic plus elastic) can also be measured by using cross head reaches a maximum before the maximum load is applied. Use
travel. The use of strain gages is recommended to obtain very the following formula to calculate the stresses beyond the
accurate data for code development. Use both axial and proportional limit:
circumferential gages. They should have an accuracy of 6 s 5 ~2/bt 2! @P2a 1 ~A/2! ~DP/D(! ~ (2!# (6)
0.005 %, preferably 6 0.001 %. Take special care in attaching
the gages to ensure that the adhesive is compatible with the where:
cladding material, the gage can measure the amount of strain DP = P2 − P1(corrected load), N
anticipated, and the adhesive can withstand the test tempera- D( = (2 − (1(corrected strain), mm/mm,
ture. An automatic data acquisition system is recommended for t = thickness, mm,
recording and evaluating the data. P = load, N, and
14.5.5 Fatigue Test: a = distance, mm.
14.5.5.1 Conduct the temperature control and measurement 14.5.6.7 Calculate the strain from the following formula:
in accordance with Practice E 139 as follows: t 5 4st/l 2 (7)
(1) Report the indicated test temperature continuously by
using a suitable device during hours when the test is unat- where:
tended. s = deflection reading, mm
(2) Indicated temperature variations along the gage length t = thickness, mm, and
of the specimens should not exceed the following limits: l = gage length, mm.
Up to 540°C, incl 62°C
14.5.6.8 Plot a stress-strain diagram using the information
540 to 1090°C, incl 63°C in 14.5.6.5-14.5.6.7.
Over 1090°C 64°C 14.5.7 Transient Test:
Overheating prior to attaining the limits specified shall not 14.5.7.1 Obtain cladding mechanical property data for
exceed 1 % above the indicated nominal test temperature; the analysis of fuel pin transient behavior under experimental
duration of such heating should not exceed 10 min. conditions in which the temperature ramps associated with
(3) Conduct strain measurement, if applicable during test, in reactor transients are simulated. The purpose of simulated
accordance with Practice E 606. transient testing of fuel cladding specimens is to define the
14.5.6 Bend Test: failure stress and strain for cladding over a wide temperature
14.5.6.1 Conduct temperature control and measurement in range for various heating rates.
accordance with Test Methods E 8. 14.5.7.2 The equipment utilized for a transient test must
14.5.6.2 Measure strain by using strain gages (room tem- provide for rapid heating of the specimen under a controlled
peratures) and a device to measure the radius of curvature in rate. Commonly, an induction generator is used with closed-
the gage section at elevated temperature. For modulus deter- loop control. A thermocouple spot-welded to the specimen or
minations, use an ASTM Type A extensometer. For routine an equivalent temperature-sensing device such as an optical
testing use ASTM Type B-1 or B-2. Optical and mechanical pyrometer provides the feedback for the control. The response
devices are acceptable for the above. rate of the temperature sensor must be rapid enough to keep
14.5.6.3 Measure the dimensions of the cross section of the pace with the various heat rates involved. During the test,
specimen to within 6 0.03 mm. monitor both the specimen pressure and temperature. Accom-
14.5.6.4 Load the specimen continuously at an initial outer plish pressure measurement conveniently with a strain-gage
fiber strain rate of 0.005 6 0.002/min at room temperature. If pressure transducer, whose output can be monitored with a
the ductility of the sample exceeds 5 %, gradually increase the recorder. Measure the temperature with the controlling device.
strain rate on subsequent tests of similar material to 0.05 6 Additional thermocouples or other temperature sensing devices
0.2/min after 0.6 % offset or 1.0 % total strain is reached. For may also be used. Generate the temperature ramps by a
elevated temperature testing, use an initial strain rate of 0.005 function generator that is calibrated to the output of the
6 0.002/min until a total strain of 1.0 % is reached and then temperature sensing device or thermocouple. All temperature
change the rate to 0.05 6 0.02/min. and pressure measuring equipment should be calibrated and
14.5.6.5 In the elastic region, the stresses induced in a should have a response time compatible with the transient.
bending beam, s, in megapascals, are given by the flexure 14.5.7.3 When induction heating is used, considerable care
formula as follows: is required in the design of the heating coil. The coil must
provide a uniform temperature along the length of the sample
s 5 3Pa/bt 2 (5)
for the duration of the test. If different heating rates are to be
where: used, different coils may be required. Insulate the coil from the
P = load, N specimen with an appropriate insert or coating.
a = distance, mm 14.5.7.4 For other heating methods, use similar cladding
b = width of gage section, mm, and temperature profiles and conditions required by 14.5.7.3.
t = thickness of gage section, mm. Conduct the test according to the following sequences:
14.5.6.6 Beyond the elastic limit or proportional limit, the (1) If using a thermocouple, spot-weld it to the specimen
stress is no longer merely a function of the load P, but rather with the wires spaced about 1.5 mm apart. Check the continuity
is a function of the variation or change in load with the change and resistance of thermocouple.

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(2) Place the specimen in the RF coil and connect the (5) Uniform elongation and method of measurement,
thermocouple and gas pressure line. Pressurize the specimen to (6) Total elongation, and
approximately 80 % of the test pressure and check for leaks. (7) Reduction of area.
(3) Heat the specimen to the desired initial temperature and 14.6.2.2 Burst Test:
adjust the pressure to the desired level. Hold the specimen at (1) Yield strength,
this temperature until equilibrium has been attained. Check all (2) Hoop strength,
equipment to make sure that the proper settings have been (3) Location of rupture with regard to any surface defects,
achieved. weld locations, or any irregularities in the tubing, and
(4) Perform the test and terminate when burst occurs. Note (4) Method by which the fuel was removed from the
readings for test time, temperature, and pressure. tubing, where applicable.
(5) After the specimen has cooled, locate the rupture and 14.6.2.3 Creep Tests:
record the location. (1) Stress in megapascals,
(6) Measure the diameter of the specimen at increments (2) Time in hours for total or plastic strains of 0.1, 0.2, 0.5,
along the axis. 1.0, and up to 5 % if available,
14.6 Report: (3) Minimum creep rate in percent per hour,
14.6.1 General—The report, regardless of the mechanical (4) Transition to third stage creep in hours,
property test, shall include the following: (5) Test duration hours indicating whether rupture oc-
14.6.1.1 Description of the material tested as recommended curred,
in 14.1, (6) Total extension for creep tests,
14.6.1.2 Description of the test specimen, size, shape, etc., (7) Elongation and reduction of area for rupture tests,
and if other than a standard specimen is used, include the data (8) Primary creep behavior,
correlating the specimen used with a standard specimen, (9) From stress-rupture curves, determine the stress to
14.6.1.3 Location and orientation of the test specimen in the rupture for times of 1, 10, 100, 1000, 10 000, and 100 000 h.
parent material, If extrapolation is involved, the report must include the ranges
14.6.1.4 Data on radiation environment as recommended in of rupture times and creep rates upon which the extrapolation
Section 4: is based, and
(1) Irradiation temperature, (10) Stress for designated creep rate of 0.000 01 and
(2) Neutron fluence, 0.0001 %/h. If extrapolation is involved, the report must
(3) Reactor location, and include the ranges of rupture times and creep rates upon which
(4) Coolant or environment. the extrapolation is based.
14.6.1.5 Trade name and model of testing machine, gripping 14.6.2.4 Fatigue Tests:
devices, extensometer, and recording devices used in the test, (1) Speed of cycling in cycle per unit time,
methods, and results of calibrations of the apparatus, (2) Description of type of control used on fatigue machine
14.6.1.6 Speed of testing, and method of measuring and and accuracy of this control,
controlling the speed, (3) Number of cycles to failure for each test condition,
14.6.1.7 Temperature of the specimen during testing, (4) S-N diagrams, if data permits or if endurance limit is
14.6.1.8 Atmosphere or medium surrounding the specimen determined,
during the test, (5) Mean stress, stress range, mean strain, and strain range,
14.6.1.9 Photographs of the fractured specimens, and
14.6.1.10 Temperature gradients and method of determina- (6) Any data or description of the test that will aid in
tion, and comparison or interpretation of data, or both,
14.6.1.11 Test specimen axial or radial restraint. 14.6.2.5 Bend Tests:
14.6.2 Specific—In addition to the information required in (1) Complete load-deflection or stress-strain curves,
14.5, the following information shall be reported for each (2) Yield strength or yield point and method of measure-
specific test: ment,
14.6.2.1 Tension Test: (3) Tensile strength, if obtained.
(1) Complete stress-strain curves (if a group of specimens 14.6.2.6 Transient Test:
exhibits similar stress-strain curves, a typical curve may be (1) Rate of heating,
reported for the group), (2) Failure temperature and pressure,
(2) Yield strength or yield point and method of measure- (3) Uniform failure strain, and
ment, (4) Environmental conditions for specimen if irradiated
(3) Tensile strength, prior to testing.
(4) Fracture strength and fracture stress. (Fracture strength
is the load at fracture divided by the initial cross-sectional area. 15. Keywords
Fracture stress is the load at fracture divided by the cross- 15.1 fuel cladding; mechanical testing; nuclear reactor fuel;
sectional area at the time of fracture.), radiation

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