ASTM G2/G2M-06(2011)e1
(Test Method)Standard Test Method for Corrosion Testing of Products of Zirconium, Hafnium, and Their Alloys in Water at 680°F (360°C) or in Steam at 750°F (400°C)
Standard Test Method for Corrosion Testing of Products of Zirconium, Hafnium, and Their Alloys in Water at 680°F (360°C) or in Steam at 750°F (400°C)
SIGNIFICANCE AND USE
5.1 This test method is primarily used as an acceptance test for products of zirconium, hafnium, and their alloys. This standard has been widely used in the development of new alloys, heat treating practices, and for evaluation of welding techniques.
5.2 Specimens are normally tested after careful etching and rinsing. Specimens with as-manufactured surfaces may also be tested without further surface removal.
5.3 When tubing with a second material clad on the inner surface is to be tested, the inner cladding shall be removed prior to the test.
SCOPE
1.1 This test method covers (1) the determination of mass gain, and (2) the surface inspection of products of zirconium, hafnium, and their alloys when corrosion tested in water at 680°F [360°C] or in steam at 750°F [400°C].
1.2 This test method is to be utilized in its entirety to the extent specified herein as a product acceptance test.
1.3 This test method may be used on wrought products, castings, powder metallurgy products, and weld metals.
1.4 Unless a single unit is used, for example corrosion mass gain in mg/dm2, the values stated in either inch-pound or SI units are to be regarded separately as standard. The values stated in each system are not exact equivalents; therefore each system must be used independently of the other. SI values cannot be mixed with inch-pound values.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see Section 9.
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Designation: G2/G2M − 06 (Reapproved 2011)
Standard Test Method for
Corrosion Testing of Products of Zirconium, Hafnium, and
Their Alloys in Water at 680°F (360°C) or in Steam at 750°F
(400°C)
This standard is issued under the fixed designation G2/G2M; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Editorial corrections were made in Section 14.3.4.1 in October 2013.
1. Scope 3. Terminology
3.1 Definitions of Terms Specific to This Standard:
1.1 This test method covers (1) the determination of mass
gain, and (2) the surface inspection of products of zirconium,
3.1.1 control coupons, n—zirconium alloy specimens of
hafnium, and their alloys when corrosion tested in water at
known performance used to monitor the validity of the test.
680°F [360°C] or in steam at 750°F [400°C].
3.1.2 etching, n—a process for removal of surface metal by
1.2 This test method is to be utilized in its entirety to the
action of acids in water.
extent specified herein as a product acceptance test.
3.1.3 GradeAwater,n—purifiedwaterhavingapHof5.0to
1.3 This test method may be used on wrought products,
8.0 and an electrical resistivity of not less than 1.0 MΩ·cm.
castings, powder metallurgy products, and weld metals.
3.1.4 Grade B water, n—water prepared with deionized or
1.4 Unlessasingleunitisused,forexamplecorrosionmass
demineralized water having a minimum electrical resistivity of
gain in mg/dm , the values stated in either inch-pound or SI
0.5 MΩ·cm.
units are to be regarded separately as standard. The values
3.1.5 ThestatedvaluesofpHandelectricalresistivityareto
stated in each system are not exact equivalents; therefore each
be met after the measured values are corrected to 77°F [25°C].
system must be used independently of the other. SI values
3.1.6 high mass gain coupons, n—zirconium alloy speci-
cannot be mixed with inch-pound values.
mens that have been specially heat-treated to produce a mass
1.5 This standard does not purport to address all of the
gain higher than the maximum specified as acceptable value
safety concerns, if any, associated with its use. It is the
used for verifying the severity of the test.
responsibility of the user of this standard to establish appro-
3.1.7 reagent grade, n—the grade of chemicals normally
priate safety and health practices and determine the applica-
used for analytical purposes.
bility of regulatory limitations prior to use. For specific
precautionary statements, see Section 9.
4. Summary of Test Method
2. Referenced Documents
4.1 Specimens of zirconium, hafnium, or their alloys are
exposed to high-pressure water or steam at elevated tempera-
2.1 ASTM Standards:
tures for 72 or 336 h. The corrosion is normally measured by
D888Test Methods for Dissolved Oxygen in Water
thegaininmassofthespecimensandbytheappearanceofthe
E29Practice for Using Significant Digits in Test Data to
oxidefilmonthespecimensurfaces.Insomeinstances,suchas
Determine Conformance with Specifications
weld evaluation, mass gain measurements are either impracti-
cal to make or not required. When so specified, appearance of
the specimen shall be the sole criterion for acceptance.
ThistestmethodisunderthejurisdictionofASTMCommitteeB10onReactive
and Refractory Metals andAlloys and is the direct responsibility of Subcommittee
B10.02 on Zirconium and Hafnium. 5. Significance and Use
Current edition approved Sept. 1, 2011. Published September 2011. Originally
5.1 This test method is primarily used as an acceptance test
approved in 1967. Last previous edition approved in 2006 as G2/G2M–06. DOI:
10.1520/G0002_G0002M-06R11E01.
for products of zirconium, hafnium, and their alloys. This
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
standard has been widely used in the development of new
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
alloys, heat treating practices, and for evaluation of welding
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. techniques.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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G2/G2M − 06 (2011)
5.2 Specimens are normally tested after careful etching and 8.9 Argon-Hydrogen Mixed Gas, for purging or controlling
rinsing. Specimens with as-manufactured surfaces may also be oxygen content.
tested without further surface removal.
9. Hazards
5.3 When tubing with a second material clad on the inner
9.1 The chemicals used in preparing specimens for this test
surface is to be tested, the inner cladding shall be removed
are hazardous. Detailed information on safe handling of
prior to the test.
organiccompounds,acidsandproductsofzirconium,hafnium,
and their alloys should be obtained from competent sources.
6. Interferences
9.2 High-temperature, high-pressure autoclave operation
6.1 Autoclave loads that have one or more specimens
must be in accordance with government regulations and
showing gross oxidation may affect results on other specimens
manufacturer’s instructions.
in the autoclave by contamination of the environment.
9.3 Hydrogen gas used for addition to the autoclave steam
7. Apparatus
supply must be handled in accordance with guidelines for
7.1 The apparatus consists of equipment for (1) etching the explosives and flammables.
specimens when required, (2) measuring the specimen surface
9.4 Donotaddcoldwaterdirectlytotheautoclavevesselin
area and mass, the water resistivity and pH, test temperature
order to accelerate cooling upon completion of testing.
and pressure, etch and rinse temperature, and (3) performing
the water or steam corrosion test at elevated temperature and
10. Sampling, Test Specimens, and Test Units
pressure.
10.1 The size and the quantity of the test specimens, the
7.1.1 Etching—An acid bath, a flowing rinse, and a deion-
method of selection, surface preparation, and test acceptance
ized water rinse are needed for proper metal removal and
criteria shall be specified in the product specification or by
stain-free rinsing. Polyethylene or polypropylene tanks are
agreement between the purchaser and the seller as stated in the
commonly used with a bottom feed for flowing water rinses.
purchase contract.
Specimen hangers are generally made of Type 300 series
10.2 Each specimen and control coupons shall be individu-
stainless steel. When many specimens are processed, a me-
ally identified.
chanical dipper for the etching process is useful.
7.1.2 Autoclaves, constructed of Type 300 series stainless
11. Preparation of Apparatus
steel or nickel base alloys such as UNS grade N06600 or
11.1 General requirements for new or reworked autoclaves
N06690andaremanufacturedtoconformtoASME(American
and parts of autoclaves previously used for testing materials
SocietyforMechanicalEngineers)andgovernmentregulations
other than to this standard are as follows:
governingunfiredpressurevessels.Theautoclaveisfittedwith
11.1.1 Before specimens are tested in a new or reworked
devices for measurement and control of pressure and
autoclave, or in one having new valves, tubing, gaskets, etc.,
temperature, safety devices, and venting valves. Control sys-
which contact the test specimen, clean the apparatus
tems for pressure and temperature adequate to meet the
thoroughly, wipe with reagent grade ethanol or acetone, and
requirements of this standard are needed. Sample holders and
rinse twice with Grade B water. Dry the autoclave or auxiliary
other internal accessories are also constructed of Type 300 or
equipmentbyvacuumcleaningordrainandwipewithaclean,
400 series stainless steel, or nickel-base alloys such as UNS
lint-free cloth, and inspect carefully to ensure freedom from
grade N06600 or N06690.
contamination.Thereshallbenovisiblecontamination,suchas
NOTE1—Ifautoclaveheatingisperformedinanoven,theovenandnot
lubricant, residues, dust or dirt, loose oxides or rust, and oil or
the autoclave will have the automatic temperature-control equipment.
grease film on the water surface, internal surface, gasket, or
7.1.3 Measuring Equipment, capable of measuring speci-
head surfaces.
–5
men dimensions to 0.002 in. [5 by 10 m] and a balance
11.1.2 Clean all new and reworked fixtures and jigs to be
–4
capable of weighing specimens to 1 by 10 g are needed.
usedintheautoclave,rinseinhotGradeBwater.Autoclavethe
fixturesandjigsforatleast1dayat750°F[400°C]in1500psi
8. Reagents and Materials
[10.3 MPa] steam or at 680°F [360°C] in water. Inspect the
8.1 Argon Gas, welding grade.
parts for corrosion product. If corrosion product is found or
electricalresistivityoftheresidualwaterafterthetestmeasures
8.2 Grade A Water.
less than 0.1 MΩ·cm, the parts should be cleaned and auto-
8.3 Grade B Water.
claved again.
8.4 Detergents and Solvents, for specimen cleaning includ-
11.2 General requirements for autoclaves and parts in con-
ing reagent grade ethanol and reagent grade acetone.
tinuous use for corrosion testing under this standard are as
8.5 Hydrofluoric Acid (HF), reagent grade.
follows:
11.2.1 With Grade B water rinse all autoclaves, fixtures,
8.6 Nitric Acid (HNO ), reagent grade.
parts, and jigs that have been in continuous use and have
8.7 Sulfuric Acid (H SO ), reagent grade.
2 4
shown satisfactory behavior in prior tests. Inspect the fixtures
8.8 Nitrogen Gas, for purging or controlling oxygen con- and jigs for corrosion products after each test and rework and
tent. re-prepare items showing loose corrosion product.
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G2/G2M − 06 (2011)
12. Calibration and Standardization 12.2.2.4 Complete the steam or water corrosion test in
accordance with any one of the four methods in 14.3.
12.1 High Mass Gain Coupon Preparation—Thesecoupons
12.2.2.5 Remove specimens and weigh in accordance with
shall be selected from a previously tested lot. The selected
the requirement of this test method.
material shall be heat treated to produce the desired mass gain.
12.2.2.6 Calculate and establish the mass gain mean and
Heatingfor8hat1652 65°F[(900 63°C]andcoolingto572
standarddeviation(n–1method)ofeachsetofcouponsforthe
6 5°F [300 6 3°C] at a rate not exceeding 6°F/min [3.3°C/
test method used.
min] will normally produce the desired mass gain.
12.2.2.7 For product acceptance tests the mean value and
12.2 Autoclaves:
standard deviation for the control coupons may be the value
12.2.1 Prior to use for product acceptance testing, an auto-
established in 12.2.2.6 or may be calculated periodically using
clave shall be profiled thermally as in 12.4.2 and shall
all accepted values determined over the preceding 3-month
demonstrate acceptability by testing at least three control
period but not less than 21 values.
coupons, one each at the top, middle, and bottom of useful
12.2.3 An alternative method for establishing the mass gain
volume. The test results shall be incorporated in the certifica-
meanandstandarddeviationforthecontrolcouponswhichare
tiondocumentfortheautoclaveacceptancetest.Whendesired,
used repeatedly is:
high mass gain coupons may also be used.
12.2.3.1 Expose the control coupons to be used in three
12.2.2 Establishing Mass Gain Mean and Standard Devia-
different tests, once each in the top, middle, and bottom of an
tion of Control Coupons—The control coupon lot and, when
autoclave, and determine mass gain.
desired, the high mass gain coupon lot mass gain mean and
12.2.3.2 Themeanvalueofeachcontrolcouponisthemean
standard deviation shall be established by a minimum of one
for the three tests.
autoclave test as follows:
12.2.3.3 Thestandarddeviationforthecontrolcouponlotis
12.2.2.1 Randomly select 12 specimens from the control
calculated by the (n–1) method using the data from all of the
coupon lot or the high mass gain coupon lot respectively.
control coupons taken from the same material lot.
12.2.2.2 Prepare all specimens per the pretest requirements
12.2.4 The new or used autoclave is considered acceptable
of this test method.
if each control coupon mass gain is reproducible within the
12.2.2.3 Locatethe12or24specimensinafixtureorjig,in
previously established control coupon mean mass gain 63
accordance with Fig. 1, and place the fixture or jig inside the
standard deviations.
useful volume of the autoclave.
12.3 Use of Control Coupons:
12.3.1 Each autoclave run used for acceptance of product
shall contain at least three control coupons with one at the top,
one at the middle, and one at the bottom of the specimen load.
12.3.2 The control coupons may be as manufactured or
etched before testing, but if etched, the surfaces should exhibit
no stains, pits, or areas of abnormal etching attack.
12.3.3 An autoclave test is considered acceptable only if
each post-test control coupon mass gain is not less than the
established mean value minus 3 standard deviations and the
visual appearance of each control coupon is equal to or better
than the product acceptance standard. If a control coupon
post-test mass gain exceeds the mean value plus 3 standard
deviations, or the specified mass gain value, and one or more
test specimens from the corresponding location in the auto-
clave failed to meet the mass gain acceptance criterion, the
failed specimen(s) may be discarded and a new test made to
determine conformance.
12.3.4 Control coupons may be reused after removal of
oxide film.
12.4 Calibration:
12.4.1 Thetemperaturemeasurementandrecordingsystems
used to determine conformance shall be calibrated at least
every 6 months and shall not deviate more than 65°F [63°C]
from calibration standards traceable to NBS or other known
national standards.
12.4.2 Vertical thermal profiles of the autoclaves at the test
temperatures shall be made at least once in each 6-month
period, or whenever the heaters or the control thermocouples
FIG. 1 Control Coupon and High Mass Gain Coupon Positioning
for Establishing Mass Gain Mean and Standard Deviation areadjustedorreplaced.Theaxialextentoftheautoclaveused
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G2/G2M − 06 (2011)
for performing the product acceptance testing shall be re- and the like. Discard or re-prepare any etched specimen
stricted to the volume shown to be within 65°F [63°C] of the exhibiting the acid stain or dull surfaces.
recorded autoclave temperature, after temperature compensa-
14.2 Dimensions, Weight, and Inspection—Measure each
tion for calibration of the thermocouples. This volume is
test specimen, either before or after testing, to 60.002 in. [65
considered the useful volume. The profile thermocouples may –5
by10 m]andcalculat
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