1、Designation: B154 121Standard Test Method forMercurous Nitrate Test for Copper Alloys1This standard is issued under the fixed designation B154; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in
2、parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1NOTEWarning statement in 1.3 was updated editorially in July 2015.1. S
3、cope*1.1 This test method describes the technique for conductingthe mercurous nitrate test for residual stresses in wroughtcopper alloy mill products.NOTE 1For any particular copper alloy, reference should be made tothe material specification.NOTE 2Test Method B858 may be considered as a possible al
4、ternativetest method which does not involve the use of mercury.NOTE 3This test method is considered historically reliable fordetermining the potential state of residual stress in copper alloys, but notpromoted for use due to the hazards relating to mercury use andenvironmentally appropriate disposal
5、.1.2 UnitsThe values stated in SI units are to be regardedas the standard. The values given in parentheses are forinformation only.1.3 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 establi
6、sh appro-priate safety and health practices and determines the applica-bility of regulatory limitations prior to use. For specificprecautionary and hazard statements see Sections 1, 6, and 7.(WarningMercury has been designated by many regulatoryagencies as a hazardous material that can cause serious
7、 medicalissues. Mercury, or its vapor, has been demonstrated to behazardous to health and corrosive to materials. Caution shouldbe taken when handling mercury and mercury containingproducts. See the applicable product Safety Data Sheet (SDS)for additional information. Users should be aware that sell
8、ingmercury and/or mercury containing products into your state orcountry may be prohibited by law.)2. Referenced Documents2.1 ASTM Standards:2B846 Terminology for Copper and Copper AlloysB858 Test Method forAmmonia Vapor Test for DeterminingSusceptibility to Stress Corrosion Cracking in CopperAlloysD
9、1193 Specification for Reagent Water3. Terminology3.1 For terms related to copper and copper alloys, refer toTerminology B846.4. Summary of Test Method4.1 The prepared test specimen is completely immersed inthe mercurous nitrate test solution for 30 min at ambienttemperature. Upon removal from the s
10、olution, the test speci-men is wiped and immediately examined visually for cracks.5. Significance and Use5.1 This test method is an accelerated test for detecting thepresence of residual (internal) stresses that might result infailure of individual parts in storage or in service due to stresscorrosi
11、on cracking.5.2 This test method is not intended for use on assemblies orparts under applied stress. If used for that purpose, the resultsshall be for information only and not a cause for rejection ofthe assembly, its component parts, or the original mill product.6. Reagents and Materials6.1 Purity
12、of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended that1This test method is under the jurisdiction of ASTM Committee B05 on Copperand Copper Alloys and is the direct responsibility of Subcommittee B05.06 onMethods of Test.Current edition approved
13、 Oct. 1, 2012. Published November 2012. Originallyapproved in 1941. Last previous edition approved in 2005 as B154 05. DOI:10.1520/B0154-12E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards vo
14、lume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1all reagents conform to the specificati
15、ons of the Committee onAnalytical Reagent of the American Chemical Society wheresuch specifications are available.3Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Purity
16、of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type IV reagent water orbetter, as defined of Specification D1193.6.3 Mercurous Nitrate SolutionThe solution shall be anaqueous mercurous nitrate solution containing 10 g of mercu-rous nitrate solution (HgNO3) and 10
17、mL of nitiric acid(HNO3) (sp gr 1.42) per litre of solution.6.4 PreparationThe aqueous mercurous nitrate solutionshall be prepared by either of the following procedures,Aor B.Used solutions may be replenished as described in 6.5.6.4.1 Procedure ADissolve 11.4 g of HgNO32H2Oor10.7 g of HgNO3H2O in ap
18、proximately 40 mL of distilledwater acidified with 10 mL of HNO3(sp gr 1.42). After thecrystals are completely dissolved, dilute the solution withwater to 1000 mL. (WarningThe mercurous nitrate crystalsare obtainable in both the monohydrate and dihydrate form andshould be handled with caution becaus
19、e of their highly toxiceffects.) (WarningWhen weighing crystals, the weight ofthe water of crystallization should be taken into consideration.The mercurous nitrate crystals are photosensitive and whenthey have turned yellow are difficult to dissolve.) (WarningCare should be exercised when handling a
20、nd mixing chemi-cals. Qualified personnel using appropriate chemical-laboratory techniques should only do the handling and mixing.)6.4.2 Procedure BDissolve 76 g of mercury in 114 mL ofdiluted HNO3(1 part water to 1 part HNO3) (sp gr 1.42).Carefully dilute with distilled water to 1000 mL. This provi
21、desa concentration of 100 g of HgNO3after a slight loss due toheating. Add the water in small portions while stirring toprevent local overdilution. This gradual dilution, together withthe excess acid, will prevent precipitation of basic salts ofmercury. Dilute 100 mL of this solution (10 %) with 7 m
22、L ofHNO3(sp gr 1.42) and 893 mL of water. (WarningMercuryis a definite health hazard and therefore equipment for thedetection and removal of mercury vapor produced in volatil-ization is recommended. The use of rubber gloves in testing isadvisable.)6.5 Replenishment of SolutionThe spent solution may
23、bereclaimed by replenishing the mercurous nitrate solution, to a1 volume percent concentration, as follows:6.5.1 Measure 50 mL of the spent HgNO3solution in agraduated cylinder.6.5.2 Transfer to an Erlenmeyer flask, and add 10 mL ofHNO3(1 + 1).6.5.3 Add slowly 1 weight per volume percent potassiumpe
24、rmanganate (KMnO4) solution from a buret with a constantshaking until there is an excess as indicated by the pink color,which persists for several minutes.6.5.4 Add iron (II) sulfate (FeSO4) crystals until thesolution, when shaken, becomes clear. Then titrate the solutionwith 0.1 N potassium thiocya
25、nate (KCNS) solution to theappearance of a reddish brown color. Repeat this procedurewith 50 mL of a standard 1 weight per volume percent ofHgNO3solution.6.5.5 The ratio, R, of the number of millilitres of KCNSsolution required to titrate the spent solution, to the number ofmillilitres required to t
26、itrate the standard solution, determinesthe number of millilitres, X, of 10 volume percent HgNO3in 3volume percent HNO3solution required to replenish 1 L ofspent solution. Values of R and X for a litre volume are givenin Table 1.7. Hazards7.1 WarningMercury is a definite health hazard in useand disp
27、osal.7.2 Suggested Mercurous Nitrate Disposal:7.2.1 To mercurous nitrate solutions add sodium hydroxide(NaOH) to pH 10 to 11.7.2.2 Filter precipitated mercury and other heavy metals.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestion
28、s on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Replenishment of Spent Merc
29、urous Nitrate Solution to1 % ConcentrationNOTE 1X = 111.1 (1 R)where:R = fraction of mercury remaining in solution (determined by titration),andX = number of millilitres of 10 volume percent mercurous nitratesolution to be added to 1 L of spent mercurous nitrate solution toraise the concentration of
30、 mercurous nitrate to 1 %.RX RX0.10 100.0 0.56 48.90.12 97.8 0.58 46.70.14 95.5 0.60 44.40.16 93.3 0.62 42.20.18 91.1 0.64 40.00.20 88.9 0.66 37.80.22 86.7 0.68 35.60.24 84.4 0.70 33.30.26 82.2 0.72 31.10.28 80.0 0.74 28.90.30 77.8 0.76 26.70.32 75.5 0.78 24.40.34 73.3 0.80 22.20.36 71.1 0.82 20.00.
31、38 68.9 0.84 17.80.40 66.7 0.86 15.60.42 64.4 0.88 13.30.44 62.2 0.90 11.10.46 60.0 0.92 8.90.48 57.8 0.94 6.70.500.520.5455.653.351.10.960.984.42.2B154 12127.2.3 Though the filtrate is low in free mercurous ormercuric ions, it must be further treated before disposal.7.2.4 To each litre of filtrate,
32、 add two drops (0.1 cm3)of24volume percent ammonium sulfide (NH4)2S.7.2.5 After the second filtering, the filtrate may be dis-carded.NOTE 4If heating is used in either of the previous procedures, thecontainer should be covered with a watch glass to prevent loss of HNO3and water to the atmosphere. Af
33、ter solution is complete, use a smallvolume of retained dilution water to rinse the watch glass into thecontainer.7.2.5.1 Monitor the filtrate to assure it meets appropriatehealth safety standards, or is disposed of properly.7.2.6 The precipitates should be collected and stored withthe mercury-conta
34、minated test samples and sold to a licensedmercury disposal-service.8. Sampling and Test Specimen Preparation8.1 The test specimen shall be prescribed in the specifica-tion for the material being tested. In the event that a testspecimen size is not prescribed in a given rod, wire, or tubespecificati
35、on, a full cross-section length of 150 mm shall betested.8.2 The presence of burrs on the test-specimen may con-tribute to acceleration of stress corrosion cracking if notremoved prior to the mercurous nitrate test.8.2.1 The burrs shall be removed by fine file or abrasivepaper to facilitate this tes
36、t.NOTE 5The presence of burrs on the test specimen may contribute toacceleration of liquid-metal embrittlement of the mercurous nitratesolution, if not removed prior to performance of the test.9. Test Procedure9.1 Degrease the specimen in a suitable alkaline degreasingsolution or organic solvent. If
37、 necessary, totally immerse thespecimen in an aqueous solution of 15 volume percent sulfuricacid (H2SO4) or 40 volume percent nitric acid until all oxidesare completely removed from its surface or pickle in suchsolutions as may be prescribed in the specification for thematerial being tested. Remove
38、the specimen from the picklingsolution and wash it immediately in running water. Drain thespecimen free of excess water and, at room temperature,immerse it totally in the mercurous nitrate solution prepared inaccordance with 6.4. Use at least 15 mL of mercurous nitratesolution per 1000 mm2of exposed
39、 surface of the test specimen.9.2 After 30 min remove the specimen from the mercurousnitrate solution. Wipe off any excess mercury from the surfaceof the specimen with damp cloth or paper towels. Immediatelyexamine it visually for cracks unless a time limitation isprovided in the product specificati
40、on.9.2.1 Tested specimens and cloth/toweling could be con-taminated with mercury and must be disposed of in accordancewith all applicable environmental regulations. They may not beincluded with returns for remelting or machined into product.9.2.2 Make sure all material including test specimens,wipin
41、g material, and mercury solutions are monitored, thatthey meet appropriate health safety handling standards, anddisposition of all related material is in accordance with allapplicable environmental regulations.9.3 Do not reuse the solution unless it is replenished to 1 %in accordance with the proced
42、ure in 6.5.10. Test Report10.1 When testing is completed by an independent third-party laboratory, the test report shall include the followinginformation. In-house captive laboratories shall only report10.1.1, 10.1.2, and 10.1.5.10.1.1 The date of test,10.1.2 Sample identification,10.1.3 Reference t
43、o the test method used,10.1.4 The number of replicate test pieces tested,10.1.5 The test results: Pass or Fail (relative to cracks) asrequired in the appropriate product specification, and10.1.6 Any other features of the material noted during thedetermination.11. Precision and Bias11.1 No statement
44、is made about the precision or bias of thistest method since the procedure is directed at a subjectivevisual interpretation of the condition of the specimen and itsrelation to an applicable product specification.12. Keywords12.1 mercurous nitrate; residual stresses; residual stress test;stress corro
45、sionB154 1213APPENDIX(Nonmandatory Information)X1.X1.1 This test method does not attempt to compare theeffectiveness of the test to other test methods, including theAmmonia Vapor Test, Test Method B858, nor does it attempt toquantify its relative effectiveness on various copper alloyproducts. These
46、issues must be addressed on a case by casebasis, since such products and tests are specific for theirrespective requirements and applications.SUMMARY OF CHANGESCommittee B05 has identified the location of selected changes to this standard since the last issue (B154 05)that may impact the use of this
47、 standard. (Approved Oct. 1, 2012.)(1) An additional mercury Warning caveat was added to 1.3.(2) Section 9 was reworded to emphasize the importance ofproper handling of mercury and the contaminated materialinvolved in the test.ASTM International takes no position respecting the validity of any paten
48、t rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision a
49、t any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the addre
