Designation: G 2/G 2M – 06

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]1
This standard is issued under the fixed designation G 2/G 2M; 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 3. Terminology
1.1 This test method covers (1) the determination of mass 3.1 Definitions of Terms Specific to This Standard:
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 Grade A water, n—purified water having a pH of 5.0
1.3 This test method may be used on wrought products, to 8.0 and an electrical resistivity of not less than 1.0 MV·cm.
castings, powder metallurgy products, and weld metals. 3.1.4 Grade B water, n—water prepared with deionized or
1.4 Unless a single unit is used, for example corrosion mass demineralized water having a minimum electrical resistivity of
gain in mg/dm2, the values stated in either inch-pound or SI 0.5 MV·cm.
units are to be regarded separately as standard. The values 3.1.5 The stated values of pH and electrical resistivity are to
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
4.1 Specimens of zirconium, hafnium, or their alloys are
2. Referenced Documents exposed to high-pressure water or steam at elevated tempera-
2.1 ASTM Standards: 2 tures for 72 or 336 h. The corrosion is normally measured by
D 888 Test Methods for Dissolved Oxygen in Water the gain in mass of the specimens and by the appearance of the
E 29 Practice for Using Significant Digits in Test Data to oxide film on the specimen surfaces. In some instances, such as
Determine Conformance with Specifications weld evaluation, mass gain measurements are either impracti-
cal to make or not required. When so specified, appearance of
1
the specimen shall be the sole criterion for acceptance.
This test method is under the jurisdiction of ASTM Committee B10 on Reactive
and Refractory Metals and Alloys and is the direct responsibility of Subcommittee 5. Significance and Use
B10.02 on Zirconium and Hafnium.
Current edition approved March 1, 2006. Published March 2006. Originally 5.1 This test method is primarily used as an acceptance test
approved in 1967. Last previous edition approved in 2002 as G 2 – 88 (2002).
2
for products of zirconium, hafnium, and their alloys. This
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
standard has been widely used in the development of new
Standards volume information, refer to the standard’s Document Summary page on alloys, heat treating practices, and for evaluation of welding
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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 G 2/G 2M – 06
5.2 Specimens are normally tested after careful etching and 9. Hazards
rinsing. Specimens with as-manufactured surfaces may also be 9.1 The chemicals used in preparing specimens for this test
tested without further surface removal. are hazardous. Detailed information on safe handling of
5.3 When tubing with a second material clad on the inner organic compounds, acids and products of zirconium, hafnium,
surface is to be tested, the inner cladding shall be removed and their alloys should be obtained from competent sources.
prior to the test. 9.2 High-temperature, high-pressure autoclave operation
must be in accordance with government regulations and
6. Interferences manufacturer’s instructions.
6.1 Autoclave loads that have one or more specimens 9.3 Hydrogen gas used for addition to the autoclave steam
showing gross oxidation may affect results on other specimens supply must be handled in accordance with guidelines for
in the autoclave by contamination of the environment. explosives and flammables.
9.4 Do not add cold water directly to the autoclave vessel in
7. Apparatus order to accelerate cooling upon completion of testing.
7.1 The apparatus consists of equipment for (1) etching the
10. Sampling, Test Specimens, and Test Units
specimens when required, (2) measuring the specimen surface
area and mass, the water resistivity and pH, test temperature 10.1 The size and the quantity of the test specimens, the
and pressure, etch and rinse temperature, and (3) performing method of selection, surface preparation, and test acceptance
the water or steam corrosion test at elevated temperature and criteria shall be specified in the product specification or by
pressure. agreement between the purchaser and the seller as stated in the
7.1.1 Etching—An acid bath, a flowing rinse, and a deion- purchase contract.
ized water rinse are needed for proper metal removal and 10.2 Each specimen and control coupons shall be individu-
stain-free rinsing. Polyethylene or polypropylene tanks are ally identified.
commonly used with a bottom feed for flowing water rinses.
Specimen hangers are generally made of Type 300 series 11. Preparation of Apparatus
stainless steel. When many specimens are processed, a me- 11.1 General requirements for new or reworked autoclaves
chanical dipper for the etching process is useful. and parts of autoclaves previously used for testing materials
7.1.2 Autoclaves, constructed of Type 300 series stainless other than to this standard are as follows:
steel or nickel base alloys such as UNS grade N06600 or 11.1.1 Before specimens are tested in a new or reworked
N06690 and are manufactured to conform to ASME (American autoclave, or in one having new valves, tubing, gaskets, etc.,
Society for Mechanical Engineers) and government regulations which contact the test specimen, clean the apparatus thor-
governing unfired pressure vessels. The autoclave is fitted with oughly, wipe with reagent grade ethanol or acetone, and rinse
devices for measurement and control of pressure and tempera- twice with Grade B water. Dry the autoclave or auxiliary
ture, safety devices, and venting valves. Control systems for equipment by vacuum cleaning or drain and wipe with a clean,
pressure and temperature adequate to meet the requirements of lint-free cloth, and inspect carefully to ensure freedom from
this standard are needed. Sample holders and other internal contamination. There shall be no visible contamination, such as
accessories are also constructed of Type 300 or 400 series lubricant, residues, dust or dirt, loose oxides or rust, and oil or
stainless steel, or nickel-base alloys such as UNS grade grease film on the water surface, internal surface, gasket, or
N06600 or N06690. head surfaces.
11.1.2 Clean all new and reworked fixtures and jigs to be
NOTE 1—If autoclave heating is performed in an oven, the oven and not
the autoclave will have the automatic temperature-control equipment. used in the autoclave, rinse in hot Grade B water. Autoclave the
fixtures and jigs for at least 1 day at 750°F [400°C] in 1500 psi
7.1.3 Measuring Equipment, capable of measuring speci- [10.3 MPa] steam or at 680°F [360°C] in water. Inspect the
men dimensions to 0.002 in. [5 by 10–5 m] and a balance parts for corrosion product. If corrosion product is found or
capable of weighing specimens to 1 by 10−4 g are needed. electrical resistivity of the residual water after the test measures
less than 0.1 MV·cm, the parts should be cleaned and auto-
8. Reagents and Materials claved again.
8.1 Argon Gas, welding grade. 11.2 General requirements for autoclaves and parts in con-
8.2 Grade A Water. tinuous use for corrosion testing under this standard are as
8.3 Grade B Water. follows:
8.4 Detergents and Solvents, for specimen cleaning includ- 11.2.1 With Grade B water rinse all autoclaves, fixtures,
ing reagent grade ethanol and reagent grade acetone. parts, and jigs that have been in continuous use and have
8.5 Hydrofluoric Acid (HF), reagent grade. shown satisfactory behavior in prior tests. Inspect the fixtures
8.6 Nitric Acid (HNO3), reagent grade. and jigs for corrosion products after each test and rework and
8.7 Sulfuric Acid (H2SO4), reagent grade. re-prepare items showing loose corrosion product.
8.8 Nitrogen Gas, for purging or controlling oxygen con-
tent. 12. Calibration and Standardization
8.9 Argon-Hydrogen Mixed Gas, for purging or controlling 12.1 High Mass Gain Coupon Preparation—These coupons
oxygen content. shall be selected from a previously tested lot. The selected

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 G 2/G 2M – 06
material shall be heat treated to produce the desired mass gain. 12.2.2.6 Calculate and establish the mass gain mean and
Heating for 8 h at 1652 6 5°F [(900 6 3°C] and cooling to 572 standard deviation (n-1 method) of each set of coupons for the
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- mean and standard deviation for the control coupons which are
tion document for the autoclave acceptance test. When desired, 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 The mean value of each control coupon is the mean
standard deviation shall be established by a minimum of one
for the three tests.
autoclave test as follows:
12.2.2.1 Randomly select 12 specimens from the control 12.2.3.3 The standard deviation for the control coupon lot is
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 Locate the 12 or 24 specimens in a fixture or jig, 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 The temperature measurement and recording systems
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
are adjusted or replaced. The axial extent of the autoclave used
for performing the product acceptance testing shall be re-
stricted to the volume shown to be within 65°F [63°C] of the
FIG. 1 Control Coupon and High Mass Gain Coupon Positioning recorded autoclave temperature, after temperature compensa-
for Establishing Mass Gain Mean and Standard Deviation tion for calibration of the thermocouples. This volume is

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 G 2/G 2M – 06
considered the useful volume. The profile thermocouples may specimens to the nearest 1 by 10−4 g with an analytical balance
be located at the center or near the radial extremity of the checked daily with a calibrated mass before use and zeroed
autoclave volume. before each fifth weighing. Do not weigh specimens until they
12.4.3 Pressure-measuring devices shall be calibrated annu- are thoroughly dry and at the same temperature as the balance.
ally and the recorded reading shall be within 650 psi 14.3 Autoclaving:
[60.35MPa] of the calibration standard over the range used for 14.3.1 Place the clean and weighed test specimens on the
testing. clean fixtures in a manner precluding specimen-to-specimen
contact. Corrosion-filmed Type 300 or 400 series stainless steel
13. Conditioning washers or wire mesh grids may be used as separators.
13.1 Test Water Quality—The water used to conduct the Immediately before immersing in the autoclave, the fixtures
corrosion test shall be Grade A water and have an oxygen containing the specimens may be rinsed in Grade B water.
content not exceeding 45 ppb. The oxygen content specifica- Immediately before operation, rinse the autoclave twice with
tion may be met either by direct measurement using the Grade B water. Place the specimens and fixtures in the useful
appropriate method in Test Methods D 888 or by the use of volume of the cleaned and rinsed autoclave.
Venting Method A or B of 14.3. 14.3.2 Venting Method A:
13.2 Autoclave Load Restrictions—The surface area of 14.3.2.1 Water Tests—Fill the clean, thoroughly rinsed au-
specimens loaded in a static autoclave shall not exceed 0.1 toclave with enough Grade A water to cover the parts being
m2/L of autoclave volume. tested during the entire test period. Calculate the amount of
13.3 Test Conditions: water to be added so that the specimens are completely
13.3.1 Temperature—The recorded temperature within the immersed in the liquid phase at the test temperature as follows:
volume used for testing shall be the specified value 65°F
Volume of water required, L 5 k~V0 2 V1!
[63°C] for steam tests and 610°F [66°C] for water tests. (1)
13.3.2 Pressure—The recorded pressure shall be as speci-
fied 6100 psig [60.7 MPa] for steam tests and 6200 psig where:
[61.4 MPa] for water tests. V0 = autoclave volume, L,
13.3.3 Time—The exposure time tolerance at the specified V1 = total volume in L of specimens and fixture, and is
temperature and pressure shall be + 8 h, − 0 h. The time at calculated by dividing the total weight in grams of
specified conditions need not be continuous. specimens and fixture by 7000.
13.3.4 Tests where temperature or pressure limits or both k = 0.8348 at 295°F [146°C],
are exceeded for not more than 10 % of the nominal test time, 0.6329 at 500°F [260°C],
but where control coupons indicate satisfactory behavior, may, 0.5954 at 550°F [288°C],
at the option of the test laboratory, be deemed acceptable. 0.5550 at 600°F [316°C],
13.4 Specimen Preparation: 0.4980 at 650°F [343°C], and
13.4.1 Etched Specimen—Specimens should be thoroughly 0.4489 at 680°F [360°C].
cleaned prior to acid etching and carefully rinsed to prepare the Add a 10 % excess of water. Activate the autoclave heating
surfaces for testing in a manner that eliminates the effects of units after the autoclave has been attached and sealed. When
machining, grinding, or other techniques used to obtain a the internal temperature reaches about 300°F [147°C], open the
specimen of the desired size. Any technique that produces the vent valve to the atmosphere or the venting manifold as
desired smooth and shiny finish free of stains may be used. necessary for sufficient time for degassing to be complete, but
Zirconium-niobium alloys etch to a matte finish. An example not to uncover the specimens and close the valve or valve
of a suitable procedure for etching and rinsing is given in manifold. Then control the autoclave for test requirements of
Appendix X1. temperature and pressure.
13.4.2 As-Manufactured Specimens—These specimens 14.3.2.2 Steam Tests—Place the fixtures and specimens in a
should be thoroughly cleaned prior to testing to avoid contami- clean, thoroughly rinsed autoclave. Add Grade A water until
nation of the autoclave which could aversely affect other the autoclave is one-fourth to three-fourths full. Activate the
specimens in the test. The extent of the specimen cleaning is autoclave heating units after the autoclave has been sealed.
often specified by agreement between contracting parties. The When the internal temperature has exceeded 230°F [110°C],
cleaning section of Appendix X1 is an example of a suitable open the vent valve to the atmosphere or the venting manifold
cleaning procedure. for sufficient time for degassing to be complete, and close the
valve. As the temperature and pressure continue to rise, open
14. Procedure and close the vent valve, as necessary, to maintain the required
14.1 Inspection of Specimens—Examine the specimens for pressure.
folds, cracks, blisters, foreign material, luster, brown acid stain, 14.3.3 Venting Method B:
and the like. Discard or re-prepare any etched specimen 14.3.3.1 Water Tests—Load the clean, thoroughly rinsed
exhibiting the acid stain or dull surfaces. autoclave with fixtures, and specimens. Fill with Grade A water
14.2 Dimensions, Weight, and Inspection—Measure each as in Venting Method A, or if autoclave is equipped with an
test specimen, either before or after testing, to 60.002 in. [65 automatic venting system, fill with enough water to cover the
by 10-5 m] and calculate the surface area rounded to the nearest specimens. Seal the autoclave and activate the heating units.
1 by 10−6 m2 in accordance with Practice E 29. Weigh the Vent the autoclave for at least 6 min after 200°F [93°C] is

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 G 2/G 2M – 06
reached. Continue to control the autoclave for the requirements as the balance for at least 1 h before weighing. Weigh the
of temperature and pressure. specimens and measure dimensions, if needed.
14.3.3.2 Steam Tests—Load the autoclave with fixtures,
15. Calculation and Interpretation of Results
specimens, and Grade A water as in Venting Method A. Seal
the autoclave and activate the heating units. The vent valve 15.1 Calculation of Mass Gain—Calculate and record the
shall be open a minimum of 10 min prior to reaching 300°F increase in specimen mass using the equation
[149°C]. As the temperature and pressure continue to rise, ~ W2 2 W1 !
DW 5 (2)
maintain the pressure at test requirements by momentarily A
opening the vent valve.
where:
14.3.4 Closed System Method C: DW = mass gain, g/m2,
14.3.4.1 Water Tests—Prepare degassed Grade A water and W1 = pre-test mass of the specimen, g,
store in a separate closed system. Place the fixtures and W2 = post-test mass of the specimen g, and
specimens in the clean, dry autoclave and assemble except for A = total surface area of the specimen, m2.
the filling connection. Evacuate the autoclave to approximately
NOTE 2—Throughout the industry the mass gain is generally reported in
10 mm Hg pressure, backfill with argon, and re-evaluate. mg/dm2.
Backfill the autoclave with argon to a gage pressure of 5 psi [34
KPa], and add the required amount of water without the 10 % 15.2 Visual Interpretation of Surfaces:
excess of Method A to the autoclave through a closed system. 15.2.1 Post-Test Specimen Visual Appearance—Examine
Then seal the autoclave and activate the heating units. No each specimen for color, luster, surface irregularities, corrosion
products, and compare against visual standards and record
venting is required.
results. Perform the visual examination in a light environment
14.3.4.2 Steam Tests—Use a procedure similar to that de- as agreed upon between the purchaser and the testing labora-
scribed in 14.3.4.1 to fill the autoclave (one-fourth to three- tory.
fourths full). After the heating units are activated, vent to attain 15.3 Invalid Tests—Any test not meeting the parameters of
the required test pressure. The autoclave is filled in a closed 12.3.3, 13.1, 13.2, and 13.3 or where the test operator can
system using degassed water. Test the Grade A water for pH, define a condition that is significantly different from that
conductivity, and oxygen content immediately before filling normally observed may be declared invalid and the test
and then record the results. repeated. Note the repeated test and the reason for it in the
14.3.5 Refreshed Autoclaving, Method D—A refreshed au- report, Section 16.
toclave with a high-pressure, constant-volume pump, a pre-
heater with controller and separate over-temperature device, 16. Report
suitable back-pressure controller, and system over-pressure 16.1 Record in the laboratory records the following infor-
protection is required. Operate the pump at rates that permit mation:
proper functioning of the pressure control system and maintain 16.1.1 Laboratory where test is performed.
the pH within 0.2 units and the electrical resistivity of the 16.1.2 Autoclave number and test date.
effluent water at 0.4 MV·cm or more. Introduce the feed water, 16.1.3 pH and resistivity of water before test.
which is initially degassed to less than 45 ppb oxygen at the 16.1.4 Test temperature, pressure, time, type of test, and
bottom of the autoclave and bleed the effluent from the top. autoclaving method.
14.3.5.1 Water Tests—Place samples in clean autoclaves 16.1.5 Mass gain, when required, and visual appearance
nearly full of Grade A water. Close the autoclave cover and remarks of each specimen and control coupon.
connect the necessary piping and instrument lines. Pump 16.1.6 Comparative criteria for visual appearance of speci-
additional Grade A water into the autoclaves until no air mens and control coupons.
bubbles come out of the open bleed-off valve. Close the
bleed-off valve and set the controller to the operating pressure. 17. Precision and Bias
When the autoclave is pressurized and the effluent water meets 17.1 Precision:
the resistivity, pH, and dissolved oxygen requirements, turn on 17.1.1 Statement on Reproducibility—An industry round
heaters, and bring the vessel to operating temperature. When robin was conducted and reported in ASTM STP 458.3 The
the test is completed, turn off the heaters, disconnect the feed interlaboratory test series using the 14-day, 750°F [400°C],
water, and cool the autoclave to less than 212°F [100°C] before 1500 psi [10.3 MPa] steam test on a single lot of Grade R60802
opening. Zircaloy yielded an average mass gain of 2.82 g/m2 with a
14.3.5.2 Steam Tests—Follow the procedure for the water standard deviation of 0.33 g/m2. Similar round robins have not
test. Autoclave blow-down through a bottom connection or dip been run on other variations of time and temperature conditions
tube is permitted if post-test water samples are not required. listed in this test method.
17.1.2 Statement on Repeatability—Table 1 tabulates the
14.4 Post-Test Measurements and Inspection—Carefully re- four laboratories reported data from at least 20 consecutive
move the specimen from the fixtures, using clean gloves or
forceps to prevent scratches. The specimens may be rinsed in
Grade B water or reagent grade ethanol and dried. Then store 3
Symposium on Application Related Phenomena in Zirconium and its Alloys,
the specimens in a clean, dry container at the same temperature ASTM STP 458, ASTM, pp 360–371.

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TABLE 1 Mass Gain Results of Repeated Tests in 750°F [400°C] specimens were exposed in each test. The as-manufactured
SteamA specimens were tubing with a belt-ground outer surface and an
Mass Gain, g/m2 inner surface that was either etched or blast abraded. Data on
3-Day Test 14-Day Test the 680°F [360°C] water test were not available in sufficient
Labor- As-Manufactured quantity to present.
atory Etched Specimens Etched Specimens
Specimens

Mean
Standard
Mean
Standard
Mean
Standard TABLE 2 High Weight Gain Coupons Data in 3- and 14-Day Tests
Deviation Deviation Deviation in 750°F [400°C] Steam
A 1.39 0.174 1.67 0.119 ... ... Weight Gain, g/m2
B 1.47 0.11 ... ... 2.62 0.15 Test
Mean Value Standard Deviation
ClB 1.65 0.106 1.71 0.057 ... ... 3-day 6.56 0.81
C2 1.60 0.142 1.60 0.047 ... ... 14-day 8.01 0.76
C3 1.69 0.147 1.64 0.087 ... ...
C4 1.61 0.074 ... ... ... ...
D 1.40 0.15 ... ... ... ...
A
One laboratory reported data on the high mass gain coupons in both the 3-
17.2 Bias—Since there is not accepted reference material
and 14-day tests in 750°F [400°C] (see Table 2). suitable for determining bias for the procedures in this test
B
Laboratory C reported data for each of four autoclaves. Other laboratories method for corrosion mass gain, no statement on bias is being
pooled data from all of their autoclaves.
made.

autoclave tests at 750°F [400°C] in steam. Each laboratory 18. Keywords

used its own test lot for the 20 consecutive tests. Three 18.1 mass gain; steam corrosion; water corrosion

APPENDIXES

(Nonmandatory Information)

X1. GUIDE TO SPECIMEN PREPARATION

X1.1 Tubes with a Second Material on Inner Diameter— X1.3.3 Generally, 0.0005 to 0.004 in. [1 by 10-5 to 1 by 10-4
When it is necessary to corrosion test such tubes, the inner m] of the surface of each coupon is removed by etching. Since
surface cladding should be completely removed to avoid the rate of metal dissolution is a function of both temperature
erroneous results due to difference in corrosion rates of the two and acid concentration, the etching rate is determined with a
materials. special test coupon before actual test specimens are etched. The
etching rate should be checked periodically when a large
X1.2 Cleaning—Clean the specimens with chemical deter- number of specimens are etched. For the zirconium-tin alloys,
gents or organic solvents. A nonmetallic brush may be used if the bath should be discarded when the etching rate is less than
required. If solvents are used, the specimens may be cleaned by 0.001 in./min [2.5 by 10-5 m/min] per surface or when a total
wiping or total immersion. Immediately after detergent clean- of 69 in.2[4.25 by 10-2 m2] of surface area per litre of acid has
ing, thoroughly rinse the test specimens in hot 120°F [49°C] been etched.
flowing water for at least 5 min. After cleaning, handle all X1.3.3.1 When etching the zirconium-niobium alloys, it is
specimens with clean, lint-free gloves. Clean the surfaces of all necessary to limit the area of specimens etched at one time to
tools, fixtures, and the like that come in contact with the clean 4.7 in.2/L [3 by 10-3 m2/L] of solution to get good surface
specimens in a manner equivalent to that used for the speci- finish, but the bath need not be discarded each time.
mens. Store all specimens so as to maintain cleanliness. X1.3.3.2 Freshly etched zirconium alloy surfaces should be
bright and lustrous and the bath should not cause preferential
X1.3 Etching: attack except at the top edge or around the holes and identifi-
X1.3.1 General—The approximate bath composition for cation marks. If preferential etching does occur elsewhere, the
unalloyed zirconium and the zirconium-tin alloys is: 3 mass % test specimen should be discarded or abraded and re-etched. If
hydrofluoric acid, 39 mass % of nitric acid, and the remainder staining does occur the specimens should be re-etched.
distilled or demineralized water. Other concentrations of re- X1.3.4 Load the test specimens on the etching fixture and
agents may be used provided the equivalent final concentra- transfer to the etching bath. (Assure that the bath temperature
tions are obtained. The etching bath temperature should not is within the limits set forth and that only the test specimens
exceed 120°F [49°C]. and hooks are immersed.) Either (a) completely withdraw and
X1.3.2 For zirconium-niobium alloys, the bath composition immerse alternately the specimens in etching fixture in the bath
is 9 6 1 % of hydrofluoric acid, 30 6 5 % of nitric acid, 30 6 at a rate of 60 cpm minimum (a cycle is defined as one
5 % of sulfuric acid, and the remainder distilled or deionized immersion and withdrawal) or (b) completely immerse the
water. This bath should be controlled to 120 to 140°F [49 to specimens on the etching fixture in the bath and agitate
60°C]. vigorously. The agitation may be accomplished by bubbling air

6
 G 2/G 2M – 06
into the etching station. Limit the total etching time to that X1.5 Final Rinse:
required to remove 0.0005 to 0.004 in. [1 by 10-5 to 1 by 10-4
X1.5.1 General—The final rinse is in Grade B water. The
m] per surface, as determined above with a test coupon.
final rinse may be performed in either a dynamic or a static
X1.4 Preliminary Rinse: system. Post-rinsing inspection will not always indicate faulty
rinsing operations. Improper techniques will be dramatically
X1.4.1 General—Test specimens should be transferred
observed at the conclusion of the corrosion test as erroneous
from the etching bath to the rinse solution as rapidly as possible
mass gains and white or generally cloudy surfaces.
to prevent staining by the acids. If any acid product remains on
the surface or is allowed to dry on the surface, the specimens X1.5.2 Dynamic System—Completely immerse the fixture
will not rinse clean and must be re-etched. and test specimens in the rinse tank which contains 175°F
X1.4.2 After etching is completed, immediately transfer the [79°C] minimum Grade B water. Monitor the outlet water for
fixture and test specimens to the first rinse tank, which contains purity. Allow the specimens to remain in the rinse long enough
cool (77°F [25°C] maximum) flowing water and completely for the effluent water to reach an electrical resistivity of 0.1
immerse for at least 5 min. The flow rate of the first rinse MV·cm, plus 5 min.
should be at least 2 bath changes per min. A bath change is X1.5.3 Static System—Rinse in flowing hot tap water and
defined as the flow rate, L/min/tank capacity in litres. If the then completely immerse the test specimens for 5 min in a tank
rinse becomes cloudy, allow the specimens to remain com- containing (195°F [91°C] minimum) Grade B water. Change
pletely immersed until the effluent water is clear. the bath whenever the electrical resistivity drops below 0.1
X1.4.2.1 If the local tap water supply is excessively hard, it MV·cm.
may be difficult to prevent precipitation of fluorides. In such
cases, preliminary rinses may be performed in flowing distilled X1.6 Drying—Cleaned or etched test specimens may be
or deionized water or in a 25 % HNO3 solution at room air-dried, wiped dry with a clean, lint-free cloth, or blown free
temperature. The preliminary rinsing of zirconium-niobium of moisture with dry air that is free of dust and acid fumes. Any
alloys must be in a 50 volume% of HNO3 solution at room of these methods may be used with or without a prior
temperature as an aid in removal of a black surface residue immersion in reagent grade alcohol. Handle cleaned and etched
(smut) which may develop during etching. Following the specimens only with forceps or clean, lint-free gloves. Keep
preliminary rinses with HNO3, rinse the specimens in flowing the test specimens in a clean container when they are not being
water. processed.

X2. RATIONALE (COMMENTARY) ON REVISION OF ASTM G 2 – 81

X2.1 The ASTM rules require a standard to be reviewed arbitrary value previously used. This change was incorporated
every five years for adequacy of technical contents. This in order to establish a more rigorous acceptance criteria and to
standard, ASTM G 2 – 81, was reviewed in 1986 and incorpo- better control the autoclave test within a run and between runs.
rates the following: X2.1.6 A method for establishing the mean and standard
X2.1.1 The title was changed from Standard Practice to deviation of control coupons has been added in this revision to
Standard Test Method since this standard is used throughout standardize the procedure. An alternate method for control
the industry as a product acceptance test. In addition the title coupons which are used repeatedly over and over is also added.
was revised to clarify the two distinct test conditions; one for X2.1.7 Requirements for reporting results was established
680°F [360°C] water and the other for 750°F [400°C] steam. in this revision.
The word “hafnium” was also added to the title. X2.1.8 The detailed sample preparation section has been
X2.1.2 The common terminology for reporting of data is moved to a nonmandatory guide in the Appendix because of
weight gain in mg/dm2. However, to conform to the ASTM wide variety of techniques used in the laboratories.
terminology, the unit of area is given in m2, the SI unit, and the X2.1.9 There remain variables affecting this test that are as
terms “weight” and “weight gain” have been replaced with yet unidentified that may lead to excessive corrosion or lack of
“mass” and“ mass gain” since the SI unit of measure is grams. corrosion. It is suspected that one of these variables is the
X2.1.3 Over the years this standard has undergone numer- presence of impurities in the water at concentration not
ous changes as well as form and style of ASTM standards. This detectable at this time. The control scheme to compensate for
revision has been restructured to follow guidelines for ASTM this feature is the presence of control coupons in the test on
test methods given in Form and Style for ASTM Standards, 7th which validity or severity of the test is measured. This control
Edition, March 1986. is imperfect because of variability in performance among
X2.1.4 Additional definitions have been added to eliminate specimens in the lot of control coupons.
confusions regarding terminologies such as control coupons X2.1.10 High weight gain coupons have been used to assure
and high weight gain coupons. minimum test sensitivity by some laboratories. This practice is
X2.1.5 The acceptance requirements for an autoclave test encouraged to form a data base consideration of the high
have been revised to be based on control coupons weight gain weight gain coupons as a mandatory requirement in future
standard deviations from the mean value rather than an revisions of this test method.

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 G 2/G 2M – 06
X2.1.11 In steam test by Venting Method A, degassing of initial water, autoclave pressure, and temperature during vent-
steam realizes in reducing the oxygen content of steam to a ing and venting duration and frequency and therefore it is
minimum level. However the venting time required to achieve impractical to specify a minimum venting time.
the desired oxygen level is dependent upon the amount of

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