1、BRITISH STANDARD BS EN ISO 9400:1996 Nickel-based alloys Determination of resistance to intergranular corrosion The European Standard EN ISO9400:1995 has the status of a BritishStandard ICS 77.060BSENISO9400:1996 This BritishStandard, having been prepared under the directionof the Engineering Sector
2、Board, was published underthe authority of the Standards Board and comesintoeffect on 15January1996 BSI 01-2000 The following BSI references relate to the work on this standard: Committee reference ISE/NFE/8 Draft for comment88/45322DC ISBN 0 580 24155 6 Committees responsible for this BritishStanda
3、rd The preparation of this BritishStandard was entrusted to Technical Committee ISE/NFE/8, Corrosion of metals and alloys, upon which the following bodies were represented: AEA Technology Aluminium Federation British Gas Plc British Non-Ferrous Metals Federation British Steel Industry Department of
4、Trade and Industry (National Physical Laboratory) Department of Transport (Transport Research Laboratory) Electricity Association Institute of Corrosion Ministry of Defence Society of Chemical Industry Welding Institute Zinc Development Association Amendments issued since publication Amd. No. Date C
5、ommentsBSENISO9400:1996 BSI 01-2000 i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 Section 1. General 1.1 Scope 3 1.2 Definition 3 1.3 Apparatus 3 1.4 Preparation of test specimens 3 1.5 Sensitization of test specimens 4 Section 2. Method A Iron(III) Sulfat
6、e Sulfuric acid test 2.1 Scope 5 2.2 Iron(III) Sulfate Sulfuric acid test solution 5 2.3 Preparation of test specimens 5 2.4 Procedure 5 2.5 Evaluation 5 Section 3. Method B Copper Copper sulfate 16% sulfuric acid test 3.1 Scope 7 3.2 Acidified copper sulfate test solution 7 3.3 Copper 7 3.4 Prepara
7、tion of test specimens 7 3.5 Procedure 7 3.6 Evaluation 7 Section 4. Method C Hydrochloric acid test 4.1 Scope 9 4.2 Hydrochloric acid test solution 9 4.3 Preparation of test specimens 9 4.4 Procedure 9 4.5 Evaluation 9 Section 5. Method D Nitric acid test 5.1 Scope 10 5.2 Nitric acid test solution
8、10 5.3 Apparatus 10 5.4 Preparation of test specimens 10 5.5 Procedure 10 5.6 Evaluation 11 Annex A (informative) Bibliography 12 Figure 1 Recommended apparatus 4 Figure 2 Alternative flask and condenser for nitric acid test 11 List of references Inside back coverBSENISO9400:1996 ii BSI 01-2000 Nati
9、onal foreword This BritishStandard has been prepared under the direction of Technical Committee ISE/NFE/8, and is the English language version of EN ISO9400:1995 Nickel-based alloys Determination of resistance to intergranular corrosion, published by the European Committee for Standardization (CEN).
10、 EN ISO9400:1995 is identical with ISO9400:1990, published by the International Organization for Standardization (ISO), and was produced as a result of international discussions in which the United Kingdom took an active part. EN ISO9400:1995 has been approved by CEN Member Bodies under the weighted
11、 voting procedures introduced in 1988 to coincide with the introduction of “New Approach” Directives from the Commission of the European Community. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct
12、application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, theEN ISO title page, pages2 to12, an inside back cover and a back cover. This standard has been upd
13、ated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO9400 November 1995 ICS 77.060 Descriptors: Nickel, nickel, alloys, corrosion, tests, corrosion tests, in
14、tergranular corrosion tests English version Nickel-based alloys Determination of resistance to intergranular corrosion (ISO9400:1990) Alliages base de nickel Dtermination de larsistance la corrosion intergranulaire (ISO9400:1990) Legierungen auf Nickelbasis Bestimmung der Bestndigkeit gegen interkri
15、stalline Korrosion (ISO9400:1990) This European Standard was approved by CEN on 1994-12-15. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date
16、lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the re
17、sponsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Nor
18、way, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1995 Copyright reserved to CEN members Ref. No. EN ISO9400:1995 EENISO9400:19
19、95 BSI 01-2000 2 Foreword The text of the International Standard from ISO/TC107, Metallic and other inorganic coatings,of the International Organization for Standardization (ISO) has been taken over as a European Standard by the Technical Committee CEN/TC262, Protection of metallic materials against
20、 corrosion. This European Standard shall be given the status ofa national standard, either by publication of an identical text or by endorsement, at the latest by May 1996. According to the CEN/CENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austr
21、ia, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, UnitedKingdom.ENISO9400:1995 BSI 01-2000 3 Section 1. General 1.1 Scope This International Standard specifies four methods for determination of the
22、susceptibility of nickel-based alloys to intergranular corrosion. These methods are for laboratory testing of susceptibility only, and a direct correlation with intergranular corrosion in actual service may not occur unless the service medium is the same as the test medium. The methods covered are a
23、s follows: Method A: iron(III) sulfate sulfuric acid test (section2); Method B: copper copper-sulfate16% sulfuric acid test (section3); Method C: hydrochloric acid test (section4); Method D: nitric acid test (section5); The appropriate method for use with a given alloy, the selection of sensitizing
24、treatment, and the acceptance criteria to be used in any evaluation have to be agreed between the buyer and seller of the alloy. As a guide, the methods specified in this International Standard should be applicable to those nickel-based alloys used for corrosion service and listed in ISO62071. 1.2 D
25、efinition For the purposes of this International Standard, the following definition applies. nickel-based alloy an alloy which includes nickel as the predominant element NOTE 1This definition is consistent with that given in ISO6372-12. 1.3 Apparatus The recommended apparatus is shown in Figure 1. T
26、he cold-finger type of condenser with standard Erlenmeyer flasks should not be used except for method D. The following items are required. 1.3.1 Four-bulb Allihn or Soxhlet condenser with45/50ground glass joint. 1.3.2 Erlenmeyer flask, capacity1dm 3 , with45/50ground glass joint. NOTE 2The use of ro
27、und flasks with a heating jacket is also acceptable. 1.3.3 Glass cradle or other equivalent means of specimen support, such as glass hooks or stirrups. The cradle should have three or four holes in it, to increase circulation of the test solution around the specimen (seeFigure 1). 1.3.4 Boiling chip
28、s to promote uniform boiling and to prevent bumping. For method A, these boiling chips should be made of pure alundum. 1.3.5 Silicone grease for application to the ground glass joint of the condenser and flask. A PTFE sleeve for the joint is also acceptable. 1.3.6 Heating device such as an electrica
29、lly heated hot-plate, for continuous boiling of the test solution. 1.3.7 Analytical balance capable of weighing to at least the nearest1mg (if mass loss is to be determined). 1.3.8 Stereoscopic microscope capable of magnification of5 to20, with a good light source, for examination of the tested spec
30、imen (for method B). 1.4 Preparation of test specimens The following requirements for the preparation of test specimens are common to all four test methods. Additional requirements are given, where necessary, in the section describing the particular method. A specimen having a total surface area of2
31、0cm 2to30cm 2is recommended. As-welded specimens should be cut so that no more than a13mm width of unaffected base metal is included on either side of the weld and heat-affected zone. It is intended to test a specimen representing as nearly as possible the surface of the material used in service. Su
32、rface finishing should be performed only as required to remove foreign material and obtain a standard, uniform finish to represent the appropriate surface, while maintaining reasonable specimen size for convenience in testing. Normally, removal of more material than necessary will have little influe
33、nce on the test results. However, in the special case of surface carburization (sometimes encountered, for instance, in tubing when carbonaceous lubricants are employed), it may only be possible to remove the carburized layer completely by heavy grinding or machining. Such treatment of non-carburize
34、d test specimens is not permissible, except in tests undertaken to demonstrate specific surface effects. When samples are cut by shearing, the deformed metal shall be removed by grinding or machining prior to testing. ENISO9400:1995 4 BSI 01-2000 Prior to testing, the test specimens shall be degreas
35、ed with a chlorine-free solvent and rinsed. 1.5 Sensitization of test specimens 1.5.1 Specimens to be given a thermal treatment prior to testing shall be clean of carbonaceous material prior to the thermal treatment. Otherwise, carburization may invalidate the test results. A light surface grinding
36、or pickling followed by washing and rinsing in a non-chlorinated solvent should provide a clean surface. It is recommended that the effect of the pickling bath on the specimen be tested prior to the environmental exposure. 1.5.2 Specimens of alloys to be given a sensitization treatment prior to test
37、ing shall be placed in a furnace at the required temperature and for the required time, and shall then be water quenched. The use of a sensitization treatment shall be agreed upon between buyer and seller. 1.5.3 Specimens of alloys that are not given a sensitization treatment shall be tested in a co
38、ndition simulating end-use conditions. Specimens from material that is intended to be welded or heat treated shall be welded or heat treated in nearly the same manner as the material will experience in fabrication or service. The specific treatment shall be agreed upon between buyer and seller. Figu
39、re 1 Recommended apparatusENISO9400:1995 BSI 01-2000 5 Section 2. Method A Iron(III) sulfate Sulfuricacid test 2.1 Scope This section describes the procedure for conducting the boiling iron(III) sulfate sulfuric acid test to determine the susceptibility of nickel-based alloys to intergranular attack
40、. 2.2 Iron(III) sulfate sulfuric acid test solution Prepare600cm 3of test solution as follows. Measure400cm 3of distilled water into a500cm 3graduated cylinder and pour into the Erlenmeyer flask(1.3.2). Measure236cm 3of reagent grade95 to98% (m/m) sulfuric acid into a250cm 3graduated cylinder. Add t
41、he acid slowly to the water in the Erlenmeyer flask to avoid boiling by the heat evolved. (Loss of vapour results in an increase in the acid concentration.) Weigh25g of reagent grade iron(III) sulfate nonahydrate Fe 2 (SO 4 ) 3 .9H 2 O, containing about75% Fe 2 (SO 4 ) 3 , and add it to the sulfuric
42、 acidsolution. A trip balance may be used. Drop several boiling chips(1.3.4) into the flask. Lubricate the ground glass joint with silicone grease(1.3.5). Fit the flask to the condenser(1.3.1) and circulate cooling water. Boil the solution until all the iron(III) sulfate is dissolved. 2.3 Preparatio
43、n of test specimens Seeclause1.4. 2.4 Procedure Measure the dimensions of the specimen to the nearest0,5mm, including the inner dimensions of any holes, and calculate the total exposed surface area. Degrease the specimen using a non-chlorinated solvent, dry and then weigh to the nearest1mg. Place th
44、e specimen in a glass cradle(1.3.3) and immerse it in boiling test solution (clause2.2). Testing of a single specimen in a flask is preferred. However, several specimens may be tested simultaneously. The number is limited only by the number of glass cradles that can be fitted into the flask (usually
45、 three or four). In no case shall different alloys be tested together. Each specimen shall be in a separate cradle so that the specimens do not touch. Mark the liquid level on the flask with a heat-resistant marker to provide a check on vapour loss. If there is an appreciable change in the level, re
46、peat the test with fresh solution and a new specimen. Continue immersion of the specimen for a period of24h or120h, then remove the specimen, rinse in water and acetone, and dry. For alloys containing less than18% chromium the exposure time is typically24h. For alloys containing more than18% chromiu
47、m the exposure time is120h. Weigh the specimen and subtract the mass from the original mass. NOTE 3No intermediate weighings are usually necessary. The tests can be run without interruption; however, if preliminary results are desired, the specimen can be removed at any time for weighing. NOTE 4No c
48、hanges in the test solution are necessary during the test period. NOTE 5Additional iron(III) sulfate inhibitor may have to be added during the test if the corrosion rate is unusually high, as evidenced by a change in the colour of the solution. More iron(III) sulfate has to be added if the total mas
49、s loss of all specimens exceeds2g during the test, iron(III) sulfate is consumed at a rate of approximately10g for each1g of dissolved metal. NOTE 6During testing, there is some deposition of iron oxides on the upper part of the Erlenmeyer flask. This can be readily removed, after completion of the test, by boiling a10% (m/m) solution of hydrochloric acid in the flask. 2.5 Evaluation 2.5.1 The effect of the test solution on the material can be measured by determining the loss of mass of the specimen. Calculate the corros
