1、Designation: G2/G2M 06 (Reapproved 2011)Standard Test Method forCorrosion Testing of Products of Zirconium, Hafnium, andTheir Alloys in Water at 680F 360C or in Steam at 750F400C1This standard is issued under the fixed designation G2/G2M; the number immediately following the designation indicates th
2、e year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers (1) the determination of m
3、assgain, and (2) the surface inspection of products of zirconium,hafnium, and their alloys when corrosion tested in water at680F 360C or in steam at 750F 400C.1.2 This test method is to be utilized in its entirety to theextent specified herein as a product acceptance test.1.3 This test method may be
4、 used on wrought products,castings, powder metallurgy products, and weld metals.1.4 Unless a single unit is used, for example corrosion massgain in mg/dm2, the values stated in either inch-pound or SIunits are to be regarded separately as standard. The valuesstated in each system are not exact equiv
5、alents; therefore eachsystem must be used independently of the other. SI valuescannot be mixed with inch-pound values.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-pria
6、te safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificprecautionary statements, see Section 9.2. Referenced Documents2.1 ASTM Standards:2D888 Test Methods for Dissolved Oxygen in WaterE29 Practice for Using Significant Digits in Test Data
7、 toDetermine Conformance with Specifications3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 control coupons, nzirconium alloy specimens ofknown performance used to monitor the validity of the test.3.1.2 etching, na process for removal of surface metal byaction of acids in wate
8、r.3.1.3 Grade A water, npurified water having a pH of 5.0to 8.0 and an electrical resistivity of not less than 1.0 MVcm.3.1.4 Grade B water, nwater prepared with deionized ordemineralized water having a minimum electrical resistivity of0.5 MVcm.3.1.5 The stated values of pH and electrical resistivit
9、y are tobe met after the measured values are corrected to 77F 25C.3.1.6 high mass gain coupons, nzirconium alloy speci-mens that have been specially heat-treated to produce a massgain higher than the maximum specified as acceptable valueused for verifying the severity of the test.3.1.7 reagent grade
10、, nthe grade of chemicals normallyused for analytical purposes.4. Summary of Test Method4.1 Specimens of zirconium, hafnium, or their alloys areexposed to high-pressure water or steam at elevated tempera-tures for 72 or 336 h. The corrosion is normally measured bythe gain in mass of the specimens an
11、d by the appearance of theoxide film on the specimen surfaces. In some instances, such asweld evaluation, mass gain measurements are either impracti-cal to make or not required. When so specified, appearance ofthe specimen shall be the sole criterion for acceptance.5. Significance and Use5.1 This te
12、st method is primarily used as an acceptance testfor products of zirconium, hafnium, and their alloys. Thisstandard has been widely used in the development of newalloys, heat treating practices, and for evaluation of weldingtechniques.1This test method is under the jurisdiction ofASTM Committee B10
13、on Reactiveand Refractory Metals and Alloys and is the direct responsibility of SubcommitteeB10.02 on Zirconium and Hafnium.Current edition approved Sept. 1, 2011. Published September 2011. Originallyapproved in 1967. Last previous edition approved in 2006 as G2/G2M 06. DOI:10.1520/G0002_G0002M-06R1
14、1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Bo
15、x C700, West Conshohocken, PA 19428-2959, United States.5.2 Specimens are normally tested after careful etching andrinsing. Specimens with as-manufactured surfaces may also betested without further surface removal.5.3 When tubing with a second material clad on the innersurface is to be tested, the i
16、nner cladding shall be removedprior to the test.6. Interferences6.1 Autoclave loads that have one or more specimensshowing gross oxidation may affect results on other specimensin the autoclave by contamination of the environment.7. Apparatus7.1 The apparatus consists of equipment for (1) etching the
17、specimens when required, (2) measuring the specimen surfacearea and mass, the water resistivity and pH, test temperatureand pressure, etch and rinse temperature, and (3) performingthe water or steam corrosion test at elevated temperature andpressure.7.1.1 EtchingAn acid bath, a flowing rinse, and a
18、deion-ized water rinse are needed for proper metal removal andstain-free rinsing. Polyethylene or polypropylene tanks arecommonly used with a bottom feed for flowing water rinses.Specimen hangers are generally made of Type 300 seriesstainless steel. When many specimens are processed, a me-chanical d
19、ipper for the etching process is useful.7.1.2 Autoclaves, constructed of Type 300 series stainlesssteel or nickel base alloys such as UNS grade N06600 orN06690 and are manufactured to conform toASME (AmericanSociety for Mechanical Engineers) and government regulationsgoverning unfired pressure vesse
20、ls. The autoclave is fitted withdevices for measurement and control of pressure and tempera-ture, safety devices, and venting valves. Control systems forpressure and temperature adequate to meet the requirements ofthis standard are needed. Sample holders and other internalaccessories are also constr
21、ucted of Type 300 or 400 seriesstainless steel, or nickel-base alloys such as UNS gradeN06600 or N06690.NOTE 1If autoclave heating is performed in an oven, the oven and notthe autoclave will have the automatic temperature-control equipment.7.1.3 Measuring Equipment, capable of measuring speci-men di
22、mensions to 0.002 in. 5 by 105m and a balancecapable of weighing specimens to 1 by 104g are needed.8. Reagents and Materials8.1 Argon Gas, welding grade.8.2 Grade A Water.8.3 Grade B Water.8.4 Detergents and Solvents, for specimen cleaning includ-ing reagent grade ethanol and reagent grade acetone.8
23、.5 Hydrofluoric Acid (HF), reagent grade.8.6 Nitric Acid (HNO3), reagent grade.8.7 Sulfuric Acid (H2SO4), reagent grade.8.8 Nitrogen Gas, for purging or controlling oxygen con-tent.8.9 Argon-Hydrogen Mixed Gas, for purging or controllingoxygen content.9. Hazards9.1 The chemicals used in preparing sp
24、ecimens for this testare hazardous. Detailed information on safe handling oforganic compounds, acids and products of zirconium, hafnium,and their alloys should be obtained from competent sources.9.2 High-temperature, high-pressure autoclave operationmust be in accordance with government regulations
25、andmanufacturers instructions.9.3 Hydrogen gas used for addition to the autoclave steamsupply must be handled in accordance with guidelines forexplosives and flammables.9.4 Do not add cold water directly to the autoclave vessel inorder to accelerate cooling upon completion of testing.10. Sampling, T
26、est Specimens, and Test Units10.1 The size and the quantity of the test specimens, themethod of selection, surface preparation, and test acceptancecriteria shall be specified in the product specification or byagreement between the purchaser and the seller as stated in thepurchase contract.10.2 Each
27、specimen and control coupons shall be individu-ally identified.11. Preparation of Apparatus11.1 General requirements for new or reworked autoclavesand parts of autoclaves previously used for testing materialsother than to this standard are as follows:11.1.1 Before specimens are tested in a new or re
28、workedautoclave, or in one having new valves, tubing, gaskets, etc.,which contact the test specimen, clean the apparatus thor-oughly, wipe with reagent grade ethanol or acetone, and rinsetwice with Grade B water. Dry the autoclave or auxiliaryequipment by vacuum cleaning or drain and wipe with a cle
29、an,lint-free cloth, and inspect carefully to ensure freedom fromcontamination.There shall be no visible contamination, such aslubricant, residues, dust or dirt, loose oxides or rust, and oil orgrease film on the water surface, internal surface, gasket, orhead surfaces.11.1.2 Clean all new and rework
30、ed fixtures and jigs to beused in the autoclave, rinse in hot Grade B water.Autoclave thefixtures and jigs for at least 1 day at 750F 400C in 1500 psi10.3 MPa steam or at 680F 360C in water. Inspect theparts for corrosion product. If corrosion product is found orelectrical resistivity of the residua
31、l water after the test measuresless than 0.1 MVcm, the parts should be cleaned and auto-claved again.11.2 General requirements for autoclaves and parts in con-tinuous use for corrosion testing under this standard are asfollows:11.2.1 With Grade B water rinse all autoclaves, fixtures,parts, and jigs
32、that have been in continuous use and haveshown satisfactory behavior in prior tests. Inspect the fixturesand jigs for corrosion products after each test and rework andre-prepare items showing loose corrosion product.12. Calibration and Standardization12.1 High Mass Gain Coupon PreparationThese coupo
33、nsshall be selected from a previously tested lot. The selectedG2/G2M 06 (2011)2material shall be heat treated to produce the desired mass gain.Heating for8hat1652 6 5F (900 6 3C and cooling to 5726 5F 300 6 3C at a rate not exceeding 6F/min 3.3C/min will normally produce the desired mass gain.12.2 A
34、utoclaves:12.2.1 Prior to use for product acceptance testing, an auto-clave shall be profiled thermally as in 12.4.2 and shalldemonstrate acceptability by testing at least three controlcoupons, one each at the top, middle, and bottom of usefulvolume. The test results shall be incorporated in the cer
35、tifica-tion document for the autoclave acceptance test. When desired,high mass gain coupons may also be used.12.2.2 Establishing Mass Gain Mean and Standard Devia-tion of Control CouponsThe control coupon lot and, whendesired, the high mass gain coupon lot mass gain mean andstandard deviation shall
36、be established by a minimum of oneautoclave test as follows:12.2.2.1 Randomly select 12 specimens from the controlcoupon lot or the high mass gain coupon lot respectively.12.2.2.2 Prepare all specimens per the pretest requirementsof this test method.12.2.2.3 Locate the 12 or 24 specimens in a fixtur
37、e or jig, inaccordance with Fig. 1, and place the fixture or jig inside theuseful volume of the autoclave.12.2.2.4 Complete the steam or water corrosion test inaccordance with any one of the four methods in 14.3.12.2.2.5 Remove specimens and weigh in accordance withthe requirement of this test metho
38、d.12.2.2.6 Calculate and establish the mass gain mean andstandard deviation (n1 method) of each set of coupons for thetest method used.12.2.2.7 For product acceptance tests the mean value andstandard deviation for the control coupons may be the valueestablished in 12.2.2.6 or may be calculated perio
39、dically usingall accepted values determined over the preceding 3-monthperiod but not less than 21 values.12.2.3 An alternative method for establishing the mass gainmean and standard deviation for the control coupons which areused repeatedly is:12.2.3.1 Expose the control coupons to be used in threed
40、ifferent tests, once each in the top, middle, and bottom of anautoclave, and determine mass gain.12.2.3.2 The mean value of each control coupon is the meanfor the three tests.12.2.3.3 The standard deviation for the control coupon lot iscalculated by the (n1) method using the data from all of thecont
41、rol coupons taken from the same material lot.12.2.4 The new or used autoclave is considered acceptableif each control coupon mass gain is reproducible within thepreviously established control coupon mean mass gain 63standard deviations.12.3 Use of Control Coupons:12.3.1 Each autoclave run used for a
42、cceptance of productshall 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 oretched before testing, but if etched, the surfaces should exhibitno stains, pits, or areas of abnorma
43、l etching attack.12.3.3 An autoclave test is considered acceptable only ifeach post-test control coupon mass gain is not less than theestablished mean value minus 3 standard deviations and thevisual appearance of each control coupon is equal to or betterthan the product acceptance standard. If a con
44、trol couponpost-test mass gain exceeds the mean value plus 3 standarddeviations, or the specified mass gain value, and one or moretest specimens from the corresponding location in the auto-clave failed to meet the mass gain acceptance criterion, thefailed specimen(s) may be discarded and a new test
45、made todetermine conformance.12.3.4 Control coupons may be reused after removal ofoxide film.12.4 Calibration:12.4.1 The temperature measurement and recording systemsused to determine conformance shall be calibrated at leastevery 6 months and shall not deviate more than 65F 63Cfrom calibration stand
46、ards traceable to NBS or other knownnational standards.12.4.2 Vertical thermal profiles of the autoclaves at the testtemperatures shall be made at least once in each 6-monthperiod, or whenever the heaters or the control thermocouplesare adjusted or replaced. The axial extent of the autoclave usedfor
47、 performing the product acceptance testing shall be re-stricted to the volume shown to be within 65F 63C of therecorded autoclave temperature, after temperature compensa-tion for calibration of the thermocouples. This volume isFIG. 1 Control Coupon and High Mass Gain Coupon Positioningfor Establishi
48、ng Mass Gain Mean and Standard DeviationG2/G2M 06 (2011)3considered the useful volume. The profile thermocouples maybe located at the center or near the radial extremity of theautoclave volume.12.4.3 Pressure-measuring devices shall be calibrated annu-ally and the recorded reading shall be within 65
49、0 psi60.35MPa of the calibration standard over the range used fortesting.13. Conditioning13.1 Test Water QualityThe water used to conduct thecorrosion test shall be Grade A water and have an oxygencontent not exceeding 45 ppb. The oxygen content specifica-tion may be met either by direct measurement using theappropriate method in Test Methods D888 or by the use ofVenting Method A or B of 14.3.13.2 Autoclave Load RestrictionsThe surface area ofspecimens loaded in a static autoclave shall not exceed 0.1m2/L of
