1、Designation: B 154 05Standard Test Method forMercurous Nitrate Test for Copper Alloys1This standard is issued under the fixed designation B 154; 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 (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method describes the technique for conductingthe me
3、rcurous nitrate test for residual stresses in wroughtcopper alloy mill products.NOTE 1For any particular copper alloy, reference should be made tothe material specification.1.2 UnitsThe values stated in SI units are to be regardedas the standard. The values given in parentheses are forinformation on
4、ly.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 establish appro-priate safety and health practices and determines the applica-bility of regulatory limitations prior to use. For specif
5、icprecautionary and hazard statements see Sections 1, 6, and 7.(WarningMercury is a definite health hazard in use anddisposal.)2. Referenced Documents2.1 ASTM Standards:2B 846 Terminology for Copper and Copper AlloysD 1193 Specification for Reagent Water3. Terminology3.1 For terms related to copper
6、and copper alloys, refer toTerminology B 846.4. 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 solution, the test speci-men is washed and immediately examined visually for crack
7、s.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 stresscorrosion cracking.5.2 This test method is not intended for use on assemblies orparts u
8、nder 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 of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise i
9、ndicated, it is intended thatall reagents conform to the specifications 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 it
10、s use without lessening the accuracy ofthe determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type IV reagent water orbetter, as defined of Specification D 1193.6.3 Mercurous Nitrate SolutionThe solution shall be anaqueous mercurous nitrate so
11、lution containing 10 g of mercu-rous nitrate solution (HgNO3) and 10 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.
12、4.1 Procedure ADissolve 11.4 g of HgNO32H2Oor10.7 g of HgNO3H2O in approximately 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 mo
13、nohydrate and dihydrate form and1This 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 Oct. 1, 2005. Published October 2005. Originallyapproved in 1941. Last previ
14、ous edition approved in 2001 as B 154 01.2For 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.3Reagent Chemicals,
15、American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions 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 Formu
16、lary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.should be handled with caution because of their highly t
17、oxiceffects.) (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 and mixing chemi-cal
18、s. 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 providesa concentration
19、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 mL ofHNO3(sp gr 1.42
20、) 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 bereclaimed by repl
21、enishing 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 potassiumpermanganate (KMnO4)
22、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 the solu-tion, when shaken, becomes clear. Then titrate the solutionwith 0.1 N potassium thiocyanate (KCNS) solut
23、ion 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 titrate the standa
24、rd 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 disposal.7.2 Suggeste
25、d 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.7.2.3 Though the filtrate is low in free mercurous ormercuric ions, it must be further treated before disposal.7.2.4 To each litre of f
26、iltrate, 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 2If 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 atmosp
27、here. After 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 mercu
28、ry-contaminated 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 tubespe
29、cification, 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
30、this test.NOTE 3The 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.TABLE 1 Replenishment of Spent Mercurous Nitrate Solution to1 % ConcentrationNOTE 1X = 111.1 (1 R)W
31、here:R = fraction of mercury remaining in solution (determined by titra-tion), 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 mercurous nitrate to 1 %.RX RX0.10 100.0 0.56 48.90.12 97.8 0
32、.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 20.00.38 68.9 0.84 17.80.40 66.7 0.86 15.60.42 64.4 0.88 13.30.44 62
33、.2 0.90 11.10.46 60.0 0.92 8.90.48 57.8 0.94 6.70.500.520.5455.653.351.10.960.984.42.2B1540529. Test Procedure9.1 Degrease the specimen in a suitable alkaline degreasingsolution or organic solvent. If necessary, totally immerse thespecimen in an aqueous solution of 15 volume percent sulfuricacid (H2
34、SO4) 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 the specimen from the picklingsolution and wash it immediately in running water. Drain thespecimen f
35、ree 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 square millimetres of exposed surface of thetest specimen.9.2 After 30 min remove the specimen from the mercurous
36、nitrate solution and wash it in running water. Wipe off anyexcess mercury from the surface of the specimen. Immediatelyexamine it visually for cracks unless a time limitation isprovided in the product specification.9.2.1 Tested specimens are mercury contaminated and mustbe disposed of properly. They
37、 may not be included with returnsfor remelting or machined into product.9.2.2 Make sure that rinse water and wiping material aremonitored to ensure that they meet appropriate health safetystandards, or are disposed of properly.9.3 Do not reuse the solution unless it is replenished to 1 %in accordanc
38、e with the procedure 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,1
39、0.1.3 Reference to 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 Bias1
40、1.1 No statement 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 stresst
41、est; stress corrosionSUMMARY OF CHANGESCommittee B05 has identified the location of selected changes to this standard since the last issue (B 154 01)that may impact the use of this standard. (Approved Oct. 1, 2005.)(1) Added Test Report section (10) and renumbered subse-quent sections.(2) Edited Sec
42、tions 1, 2, and 3 for clarity.ASTM International takes no position respecting the validity of any patent 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 in
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45、iews known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).B154053
