1、Designation: B154 05 B154 12Standard 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 num
2、ber in 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 Department of Defense.1. Scope*1.1 This test method describes the technique for conducting
3、the mercurous nitrate test for residual stresses in wrought copperalloy mill products.NOTE 1For any particular copper alloy, reference should be made to the material specification.NOTE 1For any particular copper alloy, reference should be made to the material specification.NOTE 2Test Method B858 may
4、 be considered as a possible alternative test method which does not involve the use of mercury.NOTE 3This test method is considered historically reliable for determining the potential state of residual stress in copper alloys, but not promotedfor use due to the hazards relating to mercury use and en
5、vironmentally appropriate disposal.1.2 UnitsThe values stated in SI units are to be regarded as the standard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof
6、the user of this standard to establish appropriate safety and health practices and determines the applicability of regulatorylimitations prior to use. For specific precautionary and hazard statements see Sections 1, 6, and 7.(WarningMercury is a definitehealth hazard in use and disposal.)has been de
7、signated by EPA and many state agencies as a hazardous material that can causecentral nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials.Caution should be taken when handling mercury and mercury containing products. See the applicabl
8、e product Material Safety DataSheet (MSDS) for details and EPAs website http:/www.epa.gov/mercury/faq.htm for additional information. Users should beaware that selling mercury and/or mercury containing products into your state may be prohibited by state law.)2. Referenced Documents2.1 ASTM Standards
9、:2B846 Terminology for Copper and Copper AlloysB858 Test Method for Ammonia Vapor Test for Determining Susceptibility to Stress Corrosion Cracking in Copper AlloysD1193 Specification for Reagent Water3. Terminology3.1 For terms related to copper and copper alloys, refer to Terminology B846.4. Summar
10、y of Test Method4.1 The prepared test specimen is completely immersed in the mercurous nitrate test solution for 30 min at ambient temperature.Upon removal from the solution, the test specimen is washedwiped and immediately examined visually for cracks.5. Significance and Use5.1 This test method is
11、an accelerated test for detecting the presence of residual (internal) stresses that might result in failureof individual parts in storage or in service due to stress corrosion cracking.5.2 This test method is not intended for use on assemblies or parts under applied stress. If used for that purpose,
12、 the results shallbe for information only and not a cause for rejection of the assembly, its component parts, or the original mill product.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents co
13、nform to the specifications of the Committee on Analytical Reagent of the American Chemical Society where such*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 States1specificati
14、ons are available.3 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean Type IV r
15、eagent water orbetter, as defined of Specification D1193.6.3 Mercurous Nitrate SolutionThe solution shall be an aqueous mercurous nitrate solution containing 10 g of mercurousnitrate solution (HgNO3) and 10 mL of nitiric acid (HNO3) (sp gr 1.42) per litre of solution.6.4 PreparationThe aqueous mercu
16、rous nitrate solution shall be prepared by either of the following procedures, A or B. Usedsolutions may be replenished as described in 6.5.6.4.1 Procedure ADissolve 11.4 g of HgNO32H2O or 10.7 g of HgNO3H2O in approximately 40 mL of distilled wateracidified with 10 mL of HNO3 (sp gr 1.42). After th
17、e crystals are completely dissolved, dilute the solution with water to 1000 mL.(WarningThe mercurous nitrate crystals are obtainable in both the monohydrate and dihydrate form and should be handled withcaution because of their highly toxic effects.) (WarningWhen weighing crystals, the weight of the
18、water of crystallization shouldbe taken into consideration. The mercurous nitrate crystals are photosensitive and when they have turned yellow are difficult todissolve.) (WarningCare should be exercised when handling and mixing chemicals. Qualified personnel using appropriatechemical-laboratory tech
19、niques should only do the handling and mixing.)6.4.2 Procedure BDissolve 76 g of mercury in 114 mL of diluted HNO3 (1 part water to 1 part HNO3) (sp gr 1.42). Carefullydilute with distilled water to 1000 mL. This provides a concentration of 100 g of HgNO3 after a slight loss due to heating. Addthe w
20、ater in small portions while stirring to prevent local overdilution. This gradual dilution, together with the excess acid, willprevent precipitation of basic salts of mercury. Dilute 100 mL of this solution (10 %) with 7 mL of HNO3 (sp gr 1.42) and 893mL of water. (WarningMercury is a definite healt
21、h hazard and therefore equipment for the detection and removal of mercuryvapor produced in volatilization is recommended. The use of rubber gloves in testing is advisable.)6.5 Replenishment of SolutionThe spent solution may be reclaimed by replenishing the mercurous nitrate solution, to a 1volume pe
22、rcent concentration, as follows:6.5.1 Measure 50 mL of the spent HgNO3 solution in a graduated cylinder.6.5.2 Transfer to an Erlenmeyer flask, and add 10 mL of HNO3 (1 + 1).6.5.3 Add slowly 1 weight per volume percent potassium permanganate (KMnO4) solution from a buret with a constant shakinguntil
23、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 solution, when shaken, becomes clear. Then titrate the solution with 0.1N potassium thiocyanate (KCNS) solution to the appearance of a reddish brown color. Rep
24、eat this procedure with 50 mL of astandard 1 weight per volume percent of HgNO3 solution.6.5.5 The ratio, R, of the number of millilitres of KCNS solution required to titrate the spent solution, to the number of millilitresrequired to titrate the standard solution, determines the number of millilitr
25、es, X, of 10 volume percent HgNO3 in 3 volume percentHNO3 solution required to replenish 1 L of spent solution. Values of R and X for a litre volume are given in Table 1.7. Hazards7.1 WarningMercury is a definite health hazard in use and disposal.7.2 Suggested Mercurous Nitrate Disposal:7.2.1 To mer
26、curous 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 or mercuric ions, it must be further treated before disposal.7.2.4 To each litre of filtrate, add two drops (0.1 cm 3) of 24
27、 volume percent ammonium sulfide (NH4)2S.7.2.5 After the second filtering, the filtrate may be discarded.NOTE 4If heating is used in either of the previous procedures, the container should be covered with a watch glass to prevent loss of HNO3 and waterto the atmosphere. After solution is complete, u
28、se a small volume of retained dilution water to rinse the watch glass into the container.7.2.5.1 Monitor the filtrate to assure it meets appropriate health safety standards, or is disposed of properly.7.2.6 The precipitates should be collected and stored with the mercury-contaminated test samples an
29、d sold to a licensed mercurydisposal-service.1 This test method is under the jurisdiction of ASTM Committee B05 on Copper and Copper Alloys and is the direct responsibility of Subcommittee B05.06 on Methodsof Test.Current edition approved Oct. 1, 2005Oct. 1, 2012. Published October 2005November 2012
30、. Originally approved in 1941. Last previous edition approved in 20012005as B154 01.B154 05. DOI: 10.1520/B0154-05.10.1520/B0154-12.2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume info
31、rmation, refer to the standards Document Summary page on the ASTM website.3 Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laborat
32、ory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.B154 1228. Sampling and Test Specimen Preparation8.1 The test specimen shall be prescribed in the specification for the material being tes
33、ted. In the event that a test specimen sizeis not prescribed in a given rod, wire, or tube specification, a full cross-section length of 150 mm shall be tested.8.2 The presence of burrs on the test-specimen may contribute to acceleration of stress corrosion cracking if not removed priorto the mercur
34、ous nitrate test.8.2.1 The burrs shall be removed by fine file or abrasive paper to facilitate this test.NOTE 5The presence of burrs on the test specimen may contribute to acceleration of liquid-metal embrittlement of the mercurous nitrate solution,if not removed prior to performance of the test.9.
35、Test Procedure9.1 Degrease the specimen in a suitable alkaline degreasing solution or organic solvent. If necessary, totally immerse thespecimen in an aqueous solution of 15 volume percent sulfuric acid (H2SO4) or 40 volume percent nitric acid until all oxides arecompletely removed from its surface
36、or pickle in such solutions as may be prescribed in the specification for the material beingtested. Remove the specimen from the pickling solution and wash it immediately in running water. Drain the specimen free ofexcess water and, at room temperature, immerse it totally in the mercurous nitrate so
37、lution prepared in accordance with 6.4. Useat least 15 mL of mercurous nitrate solution per 1000 squaremm2 millimetres of exposed surface of the test specimen.9.2 After 30 min remove the specimen from the mercurous nitrate solution and wash it in running water. solution. Wipe off anyexcess mercury f
38、rom the surface of the specimen. specimen with damp cloth or paper towels. Immediately examine it visually forcracks unless a time limitation is provided in the product specification.9.2.1 Tested specimens are mercury contaminated and cloth/toweling could be contaminated with mercury and must be dis
39、posedof properly. in accordance with all applicable environmental regulations. They may not be included with returns for remelting ormachined into product.9.2.2 Make sure that rinse water and wiping material are monitored to ensure all material including test specimens, wipingmaterial, and mercury s
40、olutions are monitored, that they meet appropriate health safety standards, or are disposed ofproperly.handling standards, and disposition of all related material is in accordance with all applicable environmental regulations.TABLE 1 Replenishment of Spent Mercurous Nitrate Solution to1 % Concentrat
41、ionNOTE 1X = 111.1 (1 R)Where:R = fraction of mercury remaining in solution (determined bytitration), 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 %.R X R X0.10 1
42、00.0 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 20.00.38 68.9 0.84 17.80.40 66.7 0.86 15.60
43、.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 1239.3 Do not reuse the solution unless it is replenished to 1 % in accordance with the procedure in 6.5.10. Test Report10.1 When testing is completed by an independent third-party lab
44、oratory, the test report shall include the following information.In-house captive laboratories shall only report 10.1.1, 10.1.2, and 10.1.5.10.1.1 The date of test,10.1.2 Sample identification,10.1.3 Reference to the test method used,10.1.4 The number of replicate test pieces tested,10.1.5 The test
45、results: Pass or Fail (relative to cracks) as required in the appropriate product specification, and10.1.6 Any other features of the material noted during the determination.11. Precision and Bias11.1 No statement is made about the precision or bias of this test method since the procedure is directed
46、 at a subjective visualinterpretation of the condition of the specimen and its relation to an applicable product specification.12. Keywords12.1 mercurous nitrate; residual stresses; residual stress test; stress corrosionAPPENDIX(Nonmandatory Information)X1. NEED TITLE HERE PLEASE XXXXXXXXXXXXXXXX1.1
47、 This test method does not attempt to compare the effectiveness of the test to other test methods, including the AmmoniaVapor Test, Test Method B858, nor does it attempt to quantify its relative effectiveness on various copper alloy products. Theseissues must be addressed on a case by case basis, si
48、nce such products and tests are specific for their respective requirements andapplications.SUMMARY OF CHANGESCommittee B05 has identified the location of selected changes to this standard since the last issue(B154 01B154 05) that may impact the use of this standard. (Approved Oct. 1, 2005Oct. 1, 201
49、2.)(1) Added Test Report section (An additional mercury Warning caveat10) and renumbered subsequent was added to 1.3sections(2) Edited SectionsSection 9 1,was 2, reworded to emphasize the importance of proper handling of mercury and 3 for clarity.thecontaminated material involved in the test.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, an
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