1、CEN EN*IS0*9400 95 3404589 OLL6960 T82 m BRITISH STANDARD Nickel-based alloys - Determination of resistance to intergranular corrosion The European Standard EN IS0 9400 : 1995 has the status of a British Standard Product code 00496500 BS EN IS0 9400 : 1996 BS EN IS0 9400 : 1996 Amd. No. Date Committ
2、ees responsible for this British Standard Rxt affected The preparation of this British Standard was entrusted to Rchnica Committee ISE/NFE/8, Corrosion of metals and alloys, upon which the following bodies were represented: AEA %chnology Aluminium Federation British Gas Plc British Non-Ferrous Metal
3、s Federation British Steel Industry Department of 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 T
4、his British Standard, having been prepared under the direction of the Engineering Sector Board, was published under the authority of the Standards Board and comes into effect on 15 January 1996 O BSI 1996 The following BSI references relate to the work on this standard: Committee reference iSE/NFE/B
5、 Draft for comment 88/45322 DC ISBN O 580 24155 6 CEN EN*ISO*9400 95 3404589 OLLbb2 855 BS EN IS0 9400 : 1996 Contents Committees responsible fige Inside front cover National foreword ii Foreword 2 Section 1: General 1.1 Scope 1.2 Definition 1.3 Apparatus 3 3 3 1.4 Preparation of test specimens 4 1.
6、5 Sensitization of test specimens 5 Section 2: Method A - Iron (III) Sulfate - Sulfuric acid test 2.1 Scope 6 2.2 Iron (III) Sulfate - Sulfuric acid test solution 6 2.3 Preparation of test specimens 6 2.4 Procedure 6 2.5 Evaluation 6 Section 3: Method B - Copper - Copper sulfate - 16 % sulfuric acid
7、 test 3.1 Scope 8 3.2 Acidified copper sulfate test solution 3.3 Copper 3.4 Preparation of test specimens 3.5 Procedure 3.6 Evaluation 8 Section 4 Method C - Hydrochloric acid test 4.1 Scope 4.2 Hydrochloric acid test solution 10 10 4.3 Preparation of test specimens 10 4.4 Procedure 10 4.5 Evaluatio
8、n 10 Section 5: Method D - Nitric acid test 5.1 5.2 5.3 5.4 5.5 5.6 Scope Nitric acid test solution Apparatus Preparation of test specimens Procedure 11 11 11 11 11 Evaluation 12 Annexes A (informative) Bibliography 13 Figures 1 Recommended apparatus 4 2 Alternative flask and condenser for nitric ac
9、id test 12 O BSI 1996 i CEN EN*ISO*SYOO 95 W 3904589 0118983 791 BS EN IS0 9400 : 1996 National foreword This British Standard has been prepared under the direction of Technical Committee ISE/NFE/8, and is the English language version of EN IS0 9400 : 1995 Nickel-based alloys - Determination of resi
10、stance to intergranular corrosion, published by the European Committee for Standardization (CEN). EN IS0 9400 : 1995 is identical with IS0 9400 : 1990, published by the International Organization for Standardization (ISO), and was produced as a result of international discussions in which the United
11、 Kingdom took an active Part. EN IS0 9400 : 1995 has been approved by CEN Member Bodies under the weighted voting procedures introduced in 1988 to coincide with the introduction of New Approach Directives from the Commission of the European Community. Compliance with a British Standard does not of i
12、tself confer immunity from legal obligations. ii O BSI 1996 EUROPEAN STANDARD NORMEEUROPENNE EUROPISCHE NORM EN IS0 9400 November 1995 ICs 77.060 Descriptors: nickel, nickel, alloys, corrosion, tests, corrosion tests, intergranular corrosion tests English version Nickel-based alloys - Determination
13、of resistance to intergranular corrosion (IS0 9400 : 1990) Alliages base de nickel - Dtermination de la rsistance la corrosion intergranulaire (IS0 9400 : 1990) Korrosion Legierungen auf Nickelbasis - Bestimmung der Bestndigkeit gegen interkristalline (IS0 9400 : 1990) This European Standard was app
14、roved by CEN on 1994-12-15. CEN members are bound to comply with the CENICENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national st
15、andards 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 responsibility of a CEN member into its own language and notified
16、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, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CE
17、N European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels O 1995 Copyright reserved to CEN members Ref. No. EN IS0 9400 : 1995 E - CEN EN*IS0*9400 95 D 3404589 OLLb965 5b4 m Page 2 EN IS0 9400 : 199
18、5 Foreword The text of the International Standard from ISOITC 107, Metallic and other inorganic coatings, of the International Organization for Standardization (ISO) has been taken over as a European Standard by the Technical Committee CENITC 262, Protection of metallic materials against corrosion.
19、This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by May 1996. According to the CENICENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austria, Belgium
20、, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, United Kingdom. CEN EN*IS0*9400 95 3404589 0116966 4TO Page 3 EN IS0 9400 : 1995 Nickel-based alloys - Determination of resistance to intergranular corrosion S
21、ection 1: General 1.1 Scope This International Standard specifies four methods for determinaiion of the susceptibility of nickel- based alloys to intergranular corrosion. These methods are for laboratory testing of suscep- tibility only, and a direct correlation with inier- granular corrosion in act
22、ual service may not occur unless the service medium is ihe same as the les1 medium. The melhods covered are as follows: Method A: iron(ll1) sulfate - sulfuric acid test (section 2); Method B: sulfuric acid lest (section 3); Method C: hydrochloric acid test (Section 4); Method D: nitric acid tes1 (se
23、clion 5); copper - copper-sulfate - 16 Oh The appropriate method for use with a given alloy. the selection of sensitizing treatment, and the ac- ceptance criteria to be used in any evaluation have to be agreed between the buyer and seller of lhe alloy. As a guide. lhe methods specified in this In- t
24、ernational Standard should be applicable to those nickel-based alloys used for corrosion service and listed in IS0 6207C11. 1.2 Definition For the purposes of this International Standard, the following definition applies. nickel-based alloy: An alloy which includes nickel as the predominant element.
25、 NOTE 1 IS0 6372-121. This definition is consistent with that given in 1.3 Apparatus The recommended apparatus is shown in figurei. The 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 Sox
26、hlet condenser with 45/50 ground glass joint 1.3.2 Erlenmeyer flask, capacity 1 dm3, with 45/50 ground glass joint. NOTE 2 also acceptable. The use of round flasks with a heating jacket is 1.3.3 Glass cradle or other equivalent means of specimen support. such as glass hooks or stirrups. The cradle s
27、hould have three or four holes in it, lo increase circulation of lhe test solution around the specimen (see figure 1). 1.3.4 Boiling chips to promote uniform boiling and to prevent bumping. For method A. ihese boiling chips should be made of pure alundum. 1.3.5 Silicone grease for applicalion to the
28、 ground glass joint of the condenser and flask. A PTFE sleeve for lhe joint is also acceptable 1.3.6 Heating device such as an elecirically heated hot-plale. for continuous boiling of the test solution. Page 4 EN IS0 9400 : 1995 7 1.3.7 Analytical balance capable of weighing to at least the nearest
29、1 mg (if mass loss is to be deter- mined). Use silicone stopcock grease 1.3.8 Stereoscopic microscope capable of magni- fication of 5x to 20x, with a good light source, for examination of the tested specimen (for method 8). I 11 d I I I I / Cooling water in Il II 1.4 Preparation of test specimens Th
30、e following requirements for the preparation of test specimens are common to all four test melhods. Additional requirements are given, where necess- ary, in the section describing the particular method. A specimen having a total surface area of 20 cm2 to 30 cm2 is recommended. As-welded specimens sh
31、ould be cut so that no more than a 13 mm 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. Surface finishing should be performed only as requi
32、red to remove foreign material and ob- tain a standard, uniform finish to represent the ap- propriate surface, while maintaining reasonable specimen size for convenience in testing. Normally, removal of more material than necessary will have little influence on the test reculls. However, in lhe spec
33、ial case of surface carburization (sometimes encountered, for instance, in tubing when carbonaceous lubricants are employed), it may only be possible to remove lhe carburized layer com- pletely by heavy grinding or machining. Such treat- a) Assembled apparatus Figure 1 - Recommended apparatus Dimens
34、ions in miillmeires w b) Glass cradle _ CEN EN*IS0*9400 95 3404589 OLLb968 273 Page 5 EN IS0 9400 : 1995 ment of non-carburized test specimens is no1 permissible. except in tests undertaken to demon- strate specific surface effects. When samples are cut by shearing, the deformed metal shall be remov
35、ed by grinding or machining prior to testing. Prior to testing, the test specimens shall be de- greased 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 ma- terial prior to the
36、 thermal treatment, Otherwise, carburization may invalidate the test results. A light surface grinding 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 th
37、e environmental exposure. 1.5.2 Specimens of alloys to be given a sensitization treatment prior to testing shall be placed in a furnace at the required temperature and lor the required time. and shall then be water quenched. The use of a sensitization treatment shall be agreed upon between buyer and
38、 seller. 1.5.3 Specimens of alloys that are not given a sensitization treatment shall be tested in a condition simulating end-use conditions. Specimens from ma- terial that is intended to be welded or heat treated shall be welded or heat treated in nearly the same manner as the material will experie
39、nce in abri- cation or service. The specific treatment shall be agreed upon between buyer and seller. . CEN EN*ISO*7400 75 340q587 0LLb969 LOT Page 6 EN IS0 9400 : 1995 Section 2: Method A - Iron(ll1) sulfate - Sulfuric acid test 2.1 Scope This section describes the procedure for conducting the boil
40、ing iron(l1l) sulfate - sulfuric acid test to de- termine the susceptibility of nickel-based alloys to intergranular attack. 2.2 Iron(ll1) sulfate - sulfuric acid test solution Prepare 600 cm3 of test solution as follows. Measure 400 cm3 of distilled water into a 500 cm3 graduated cylinder and pour
41、into the Erlenmeyer flask (1.3.2). Measure 236 cm3 of reagent grade 95 to 98 YO (nt/rn) sulfuric acid into a 250 cm3 graduated cylinder. Add the 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.) W
42、eigh 25 g of reagent grade iron(l1l) sulfate nona hydrate Fe,(SO,),.SH,O, conta in ng a bout 75 Oh Fe,(SO,), 3. and add it to the sulfuric acid sol- ution. 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). Fi
43、t the flask to the condenser (1.3.1) and circulate cooling water. Boil the solution until all the iron(ll1) sulfate is dis- solved. 2.3 Preparation of test specimens See clause 1.4 2.4 Procedure Measure the dimensions of lhe specimen to the nearest 0,5 mm, including the inner dimensions of any holes
44、, and calculate the tola1 exposed surface area. Degrease the specimen using a non-chlorinated solvent, dry and then weigh to the nearest 1 mg. Place the specimen in a glass cradle (1.3.3) and im- merse it in boiling test solution (clause 2.2;. Testing of a single specimen in a flask is preferred. Ho
45、wever, several specimens may be tested simul- taneously. The number is limited only by the number of glass cradles that can be fitted into the flask (usually three or four). In no case shall different al- loys be tested together. Each specimen shall be in a separate cradle so that the specimens do n
46、ot 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, repeat the test with fresh solution and a new specimen. Conlinue immersion of the specimen for a period of 24 h or 120 h, then remove lhe spec
47、imen, rinse in water and acetone, and dry. For alloys containing less than 18 O/O chromium the exposure time is typi- cally 24 h. For alloys containing more than 18 % chromium the exposure time is 120 h. Weigh lhe specimen and subtract the mass from the original mass. NOTES 3 No intermediate weighin
48、gs are usually necessary. The tests can be run without interruption; however, if prelimi- nary resulls are desired, the specimen can be removed at any time for weighing. 4 the test period. No changes in the test solution are necessary during 5 Additional iron(l1l) sulfate inhibitor may have to be ad
49、ded during the test if the corrosion rate is unusually high, as evidenced by a change in the colour of the sol- ution. More iron(ll1) sulfate has to be added if the total mass loss of all specimens exceeds 2 g during the test, iron(il1) sulfate is consumed al a rate of approximately 10 g for each 1 g of dissolved metal 6 During lesting. 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 a 10 % (mim) solution of hydrochlo
