ASTM G2/G2M-06(2011)

Standard Test Method for Corrosion Testing of Products of Zirconium, Hafnium, and Their Alloys in Water at 680<span class='unicode'>&#x00B0;</span>F [360<span class='unicode'>&#x00B0;</span>C] or in Steam at 750<span class='unicode'>&#x00B0;</span>F [400<

SIGNIFICANCE AND USE
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.
Specimens are normally tested after careful etching and rinsing. Specimens with as-manufactured surfaces may also be tested without further surface removal.
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.

General Information

• Status: Historical
• Publication Date: 31-Aug-2011
• ICS: 77.060 - Corrosion of metals
• ICS: 77.120.99 - Other non-ferrous metals and their alloys
• Technical Committee: B10 - Reactive and Refractory Metals and Alloys
• Drafting Committee: B10.02 - Zirconium and Hafnium

Relations

• Replaces: ASTM G2/G2M-06 - Standard Test Method for Corrosion Testing of Products of Zirconium, Hafnium, and Their Alloys in Water at 680&#176;F [360&#176;C]or in Steam at 750&#176;F [400&#176;C]
• Effective Date: 01-Sep-2011
• Replaced By: ASTM G2/G2M-06(2011)e1 - Standard Test Method for Corrosion Testing of Products of Zirconium, Hafnium, and Their Alloys in Water at 680&deg;F (360&deg;C) or in Steam at 750&deg;F (400&deg;C)
• Effective Date: 01-Sep-2011
• Referred By: ASTM B811-13(2022)e1 - Standard Specification for Wrought Zirconium Alloy Seamless Tubes for Nuclear Reactor Fuel Cladding
• Effective Date: 01-Sep-2011
• Referred By: ASTM B352/B352M-17(2021) - Standard Specification for Zirconium and Zirconium Alloy Sheet, Strip, and Plate for Nuclear Application
• Effective Date: 01-Sep-2011
• Referred By: ASTM B353-12(2022)e1 - Standard Specification for Wrought Zirconium and Zirconium Alloy Seamless and Welded Tubes for Nuclear Service (Except Nuclear Fuel Cladding)
• Effective Date: 01-Sep-2011
• Referred By: ASTM B351/B351M-13(2023) - Standard Specification for Hot-Rolled and Cold-Finished Zirconium and Zirconium Alloy Bars, Rod, and Wire for Nuclear Application
• Effective Date: 01-Sep-2011

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: G2/G2M − 06 (Reapproved2011)
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.
1. Scope 3.1.1 control coupons, n—zirconium alloy specimens of
known performance used to monitor the validity of the test.
1.1 This test method covers (1) the determination of mass
3.1.2 etching, n—a process for removal of surface metal by
gain, and (2) the surface inspection of products of zirconium,
action of acids in water.
hafnium, and their alloys when corrosion tested in water at
680°F [360°C] or in steam at 750°F [400°C].
3.1.3 GradeAwater,n—purifiedwaterhavingapHof5.0to
8.0 and an electrical resistivity of not less than 1.0 MΩ·cm.
1.2 This test method is to be utilized in its entirety to the
extent specified herein as a product acceptance test. 3.1.4 Grade B water, n—water prepared with deionized or
demineralized water having a minimum electrical resistivity of
1.3 This test method may be used on wrought products,
0.5 MΩ·cm.
castings, powder metallurgy products, and weld metals.
3.1.5 ThestatedvaluesofpHandelectricalresistivityareto
1.4 Unlessasingleunitisused,forexamplecorrosionmass
2 be met after the measured values are corrected to 77°F [25°C].
gain in mg/dm , the values stated in either inch-pound or SI
3.1.6 high mass gain coupons, n—zirconium alloy speci-
units are to be regarded separately as standard. The values
mens that have been specially heat-treated to produce a mass
stated in each system are not exact equivalents; therefore each
gain higher than the maximum specified as acceptable value
system must be used independently of the other. SI values
used for verifying the severity of the test.
cannot be mixed with inch-pound values.
3.1.7 reagent grade, n—the grade of chemicals normally
1.5 This standard does not purport to address all of the
used for analytical purposes.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 Specimens of zirconium, hafnium, or their alloys are
bility of regulatory limitations prior to use. For specific
exposed to high-pressure water or steam at elevated tempera-
precautionary statements, see Section 9.
tures for 72 or 336 h. The corrosion is normally measured by
thegaininmassofthespecimensandbytheappearanceofthe
2. Referenced Documents
oxidefilmonthespecimensurfaces.Insomeinstances,suchas
2.1 ASTM Standards:
weld evaluation, mass gain measurements are either impracti-
D888Test Methods for Dissolved Oxygen in Water
cal to make or not required. When so specified, appearance of
E29Practice for Using Significant Digits in Test Data to
the specimen shall be the sole criterion for acceptance.
Determine Conformance with Specifications
5. Significance and Use
3. Terminology
5.1 This test method is primarily used as an acceptance test
3.1 Definitions of Terms Specific to This Standard:
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
ThistestmethodisunderthejurisdictionofASTMCommitteeB10onReactive
techniques.
and Refractory Metals andAlloys and is the direct responsibility of Subcommittee
B10.02 on Zirconium and Hafnium.
5.2 Specimens are normally tested after careful etching and
Current edition approved Sept. 1, 2011. Published September 2011. Originally
rinsing. Specimens with as-manufactured surfaces may also be
approved in 1967. Last previous edition approved in 2006 as G2/G2M–06. DOI:
tested without further surface removal.
10.1520/G0002_G0002M-06R11.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.3 When tubing with a second material clad on the inner
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
surface is to be tested, the inner cladding shall be removed
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. prior to the test.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
G2/G2M − 06 (2011)
6. Interferences organiccompounds,acidsandproductsofzirconium,hafnium,
and their alloys should be obtained from competent sources.
6.1 Autoclave loads that have one or more specimens
showing gross oxidation may affect results on other specimens 9.2 High-temperature, high-pressure autoclave operation
in the autoclave by contamination of the environment. must be in accordance with government regulations and
manufacturer’s instructions.
7. Apparatus
9.3 Hydrogen gas used for addition to the autoclave steam
supply must be handled in accordance with guidelines for
7.1 The apparatus consists of equipment for (1) etching the
specimens when required, (2) measuring the specimen surface explosives and flammables.
area and mass, the water resistivity and pH, test temperature
9.4 Donotaddcoldwaterdirectlytotheautoclavevesselin
and pressure, etch and rinse temperature, and (3) performing
order to accelerate cooling upon completion of testing.
the water or steam corrosion test at elevated temperature and
pressure.
10. Sampling, Test Specimens, and Test Units
7.1.1 Etching—An acid bath, a flowing rinse, and a deion-
10.1 The size and the quantity of the test specimens, the
ized water rinse are needed for proper metal removal and
method of selection, surface preparation, and test acceptance
stain-free rinsing. Polyethylene or polypropylene tanks are
criteria shall be specified in the product specification or by
commonly used with a bottom feed for flowing water rinses.
agreement between the purchaser and the seller as stated in the
Specimen hangers are generally made of Type 300 series
purchase contract.
stainless steel. When many specimens are processed, a me-
chanical dipper for the etching process is useful.
10.2 Each specimen and control coupons shall be individu-
7.1.2 Autoclaves, constructed of Type 300 series stainless ally identified.
steel or nickel base alloys such as UNS grade N06600 or
N06690andaremanufacturedtoconformtoASME(American 11. Preparation of Apparatus
SocietyforMechanicalEngineers)andgovernmentregulations
11.1 General requirements for new or reworked autoclaves
governingunfiredpressurevessels.Theautoclaveisfittedwith
and parts of autoclaves previously used for testing materials
devices for measurement and control of pressure and
other than to this standard are as follows:
temperature, safety devices, and venting valves. Control sys-
11.1.1 Before specimens are tested in a new or reworked
tems for pressure and temperature adequate to meet the
autoclave, or in one having new valves, tubing, gaskets, etc.,
requirements of this standard are needed. Sample holders and
which contact the test specimen, clean the apparatus
other internal accessories are also constructed of Type 300 or
thoroughly, wipe with reagent grade ethanol or acetone, and
400 series stainless steel, or nickel-base alloys such as UNS
rinse twice with Grade B water. Dry the autoclave or auxiliary
grade N06600 or N06690.
equipmentbyvacuumcleaningordrainandwipewithaclean,
lint-free cloth, and inspect carefully to ensure freedom from
NOTE1—Ifautoclaveheatingisperformedinanoven,theovenandnot
the autoclave will have the automatic temperature-control equipment.
contamination.Thereshallbenovisiblecontamination,suchas
lubricant, residues, dust or dirt, loose oxides or rust, and oil or
7.1.3 Measuring Equipment, capable of measuring speci-
–5
grease film on the water surface, internal surface, gasket, or
men dimensions to 0.002 in. [5 by 10 m] and a balance
–4
head surfaces.
capable of weighing specimens to 1 by 10 g are needed.
11.1.2 Clean all new and reworked fixtures and jigs to be
usedintheautoclave,rinseinhotGradeBwater.Autoclavethe
8. Reagents and Materials
fixturesandjigsforatleast1dayat750°F[400°C]in1500psi
8.1 Argon Gas, welding grade.
[10.3 MPa] steam or at 680°F [360°C] in water. Inspect the
8.2 Grade A Water.
parts for corrosion product. If corrosion product is found or
electricalresistivityoftheresidualwaterafterthetestmeasures
8.3 Grade B Water.
less than 0.1 MΩ·cm, the parts should be cleaned and auto-
8.4 Detergents and Solvents, for specimen cleaning includ-
claved again.
ing reagent grade ethanol and reagent grade acetone.
11.2 General requirements for autoclaves and parts in con-
8.5 Hydrofluoric Acid (HF), reagent grade.
tinuous use for corrosion testing under this standard are as
8.6 Nitric Acid (HNO ), reagent grade.
follows:
11.2.1 With Grade B water rinse all autoclaves, fixtures,
8.7 Sulfuric Acid (H SO ), reagent grade.
2 4
parts, and jigs that have been in continuous use and have
8.8 Nitrogen Gas, for purging or controlling oxygen con-
shown satisfactory behavior in prior tests. Inspect the fixtures
tent.
and jigs for corrosion products after each test and rework and
8.9 Argon-Hydrogen Mixed Gas, for purging or controlling re-prepare items showing loose corrosion product.
oxygen content.
12. Calibration and Standardization
9. Hazards
12.1 High Mass Gain Coupon Preparation—Thesecoupons
9.1 The chemicals used in preparing specimens for this test shall be selected from a previously tested lot. The selected
are hazardous. Detailed information on safe handling of material shall be heat treated to produce the desired mass gain.
G2/G2M − 06 (2011)
Heatingfor8hat1652 65°F[(900 63°C]andcoolingto572 12.2.2.6 Calculate and establish the mass gain mean and
6 5°F [300 6 3°C] at a rate not exceeding 6°F/min [3.3°C/ standarddeviation(n–1method)ofeachsetofcouponsforthe
min] will normally produce the desired mass gain. test method used.
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
standard deviation shall be established by a minimum of one 12.2.3.2 Themeanvalueofeachcontrolcouponisthemean
autoclave test as follows: for the three tests.
12.2.2.1 Randomly select 12 specimens from the control 12.2.3.3 Thestandarddeviationforthecontrolcouponlotis
coupon lot or the high mass gain coupon lot respectively.
calculated by the (n–1) method using the data from all of the
12.2.2.2 Prepare all specimens per the pretest requirements control coupons taken from the same material lot.
of this test method.
12.2.4 The new or used autoclave is considered acceptable
12.2.2.3 Locatethe12or24specimensinafixtureorjig,in
if each control coupon mass gain is reproducible within the
accordance with Fig. 1, and place the fixture or jig inside the
previously established control coupon mean mass gain 63
useful volume of the autoclave.
standard deviations.
12.2.2.4 Complete the steam or water corrosion test in
12.3 Use of Control Coupons:
accordance with any one of the four methods in 14.3.
12.3.1 Each autoclave run used for acceptance of product
12.2.2.5 Remove specimens and weigh in accordance with
shall contain at least three control coupons with one at the top,
the requirement of this test method.
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
areadjustedorreplaced.Theaxialextentoftheautoclaveused
for performing the product acceptance testing shall be re-
stricted to the volume shown to be within 65°F [63°C] of the
recorded autoclave temperature, after temperature compensa-
FIG. 1 Control Coupon and High Mass Gain Coupon Positioning
for Establishing Mass Gain Mean and Standard Deviation tion for calibration of the thermocouples. This volume is
G2/G2M − 06 (2011)
–5
considered the useful volume. The profile thermocouples may by10 m]andcalculatethesurfacearearoundedtothenearest
–6 2
be located at the center or near the radial extremity of the 1by10 m in accordance with Practice E29. Weigh the
–4
autoclave volume. specimenstothenearest1by10 gwithananalyticalbalance
12.4.3 Pressure-measuring devices shall be calibrated annu- checked daily with a calibr
...