1、 CEN EN*ISO 9455-9 95 m 340Y589 OLL9L3L bTb m BRITISH STANDARD Soft soldering fluxes - Test methods Part 9. Determination of ammonia content The European Standard EN IS0 9455-9 : 1995 has the status of a British Standard ICs 25.160.20; 25.160.50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED
2、BY COPYRIGHT LAM BS EN IS0 3455-9 : 1996 BS EN IS0 9455-9 : 1996 Amd. No. Committees responsible for this British Standard Date Text affected The preparation of this British Standard was entrusted to Technical Committee Nm7, lin and tin alloys, upon which the following bodies were represented Associ
3、ation of British Pewter Craftsmen British Iron and Steel Producers Association Federation of the Electronics Industry International Tin Research Institute London Metal Exchange Metal Packaging Manufacturers Association Solder Makers Association Co-opted members The following bodies were also represe
4、nted in the drafhng of the standard, through subcommittees and panels: British Plumbing Fittings Manufacturers Association Institute of Metal Finishing Ministry of Defence Co-opted members This British Standard, having been prepared under the direction of the Engineering Sector Board, was published
5、under the authority of the Standards Board and comes into effect on 15 Februm 1996 O BSI 1996 The following BSI references relate to the work on this standard Committee reference NFEY27 Draft for comment 92/42775 DC I I ISBN O 680 25230 2 CEN ENWISO 9L155-9 95 = 3404589 OLL9133 479 BS EN IS0 9455-9
6、: 1996 Contents Committees responsible National foreword page Inside front cover ii Foreword Method 1 Scope 2 Normative reference 3 Principle 4 Reagents 5 Apparatus 6 Procedure 7 Calculation of results 8 Precision 9 Test report 2 2 3 3 3 3 4 4 5 5 6 Annex ZA (normative) Normative references to inter
7、national publications with their relevant EuroDean Dublications 7 Figure 1 Apparatus for determination of ammonia content 4 O BSI 1996 i - - CEN EN*ISO 7455-9 95 m 3404589 OLL9L34 305 m BS EN IS0 9455-9 : 1996 National foreword This British Standard has been prepared by Technical Committee NFE/27 an
8、d is the English language version of EN IS0 94559 : 1995 Soj SolderingJZwes - Test methods -Part 9: Determination of ammonia content, published by the European Committee for Standardization (CEN). EN IS0 94559 : 1995 is identical with IS0 94559 : 1993, published by the international Organization for
9、 Standardization (ISO). Cross-reference Publication referred to Corresponding British Standard BS EN 29454 Soft solderingJuxes Clms.cation and requirements Part 1 : 1994 C.!msification, labelling and pachzgirq IS0 9454-1 : 1990 Compliance with a British Standard does not of itself confer immunity fr
10、om legal obligations. ii O BSI 1996 CEN ENxISO 9455-9 95 M 3404589 OLL9135 241 EUROPEAN STBARD NORME EUROPENNE EUROPmE NORM EN IS0 94559 September 1995 ICs 25.160.20; 25.160.50 Descriptors: Soldering, soldering fluxes, tests, chemical analysis, determination of content, ammonia (gas), volumetric ana
11、lysis English version Soft soldering fluxes - Test methods - Part 9 Deterrnjnation of ammonia content (IS0 94559 : 1993) Flux de brasage tendre - Mthodes dessai - Partie 9: Dosage de lammoniac Flumittel zum Weichlten - PrUfverfahren - Teil 9 Bestimmung des Ammoniumgehaltes (IS0 9455-9 : 1993) (IS0 9
12、455-9 : 1993) This European Standard was approved by CEN on 1995-08-27. CEN members are bound to comply with the CENKENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any akeration. Up-to-date lists and bibliographi
13、cal 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 responsibility of a CEN
14、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, Norway, Portugal, Spain,
15、Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fur Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels O 1995 All rights of reproduction and communication in any form and by any means reserved in ali
16、countries to CEN and its members. Ref. No. EN IS0 9455-9 : 1995 E CEN ENkISO 9455-9 95 M 3404589 Ol119L36 LBB M Page 2 EN IS0 9455-9 : 1995 Foreword The text of the International Standard from ISOAC 44, Welding and allied processes, of the International Organization for Standardization OSO) has been
17、 taken over as a European Standard by the Technical Committee CEN/TC 121, Weldmg. 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 March 1996, and conflicting national standards sha be withdrawn at
18、 the latest by March 1996. According to the CENKENELEC Internal Regulations, the following countries are bound to implement this European Standard Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerla
19、nd, United Kingdom. NOTE. Normative references to International Standards are listed in annex ZA (normative). O BSI 1996 CEN ENUISO 9455-9 95 W 3404589 0119137 014 W Page 3 EN IS0 9455-9 : 1995 Soft soldering fluxes - Test methods - Part 9: Determination of ammonia content 1 Scope This part of IS0 9
20、455 specifies a distillation method for the determination of the ammonia content of solid, paste or liquid fluxes. The method is applicable to fluxes of class 3.1.1 only, as defined in IS0 9454-1. 2 Normative reference The following standard contains provisions which, through reference in this text,
21、 constitute provisions of this part of IS0 9455. At the time of publication, the edition indicated was valid. All standards are subject to revision, and parties to agreements based on this part of IS0 9455 are encouraged to investigate the possibility of applying the most recent edition of the stand
22、ard indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 9454-1 : 1990, Soft soldering fluxes - Classi- fication and requirements - Part 1: Classification, labelling and packaging. 3 Principle The prepared flux solution is distilled with sodium h
23、y- droxide to expel the ammonia present in the flux. The resulting distillate is passed into a standard sulfuric acid solution. The excess acid is then titrated with sodium hydroxide solution and the ammonia content of the flux is calculated. 4 Reagents 4.1 General Use only reagents of recognized an
24、alytical quality and only distilled, or deionized, water. 4.2 Sodium hydroxide solution, 1 ,O mol/l standard solution, commercially available. Alternatively, use an approximately 1 ,O mol/l solution of sodium hydroxide, prepared by the following method. Dissolve 40 g of sodium hydroxide in water and
25、 cool. Transfer the solution to a 1 litre volumetric flask, dilute to the mark and mix well. Standardize this solution with 0.5 mol/l sulfuric acid solution (4.3). 4.3 Sulfuric acid, 0,5 mol/l, standard solution, com- mercially available. Alternatively, use an approximately 0,5 mol/l solution of sul
26、furic acid prepared by the following method. Cautiously add 30 ml of sulfuric acid (e = 1,84 g/ml) to 400 ml of water and mix. Cool and transfer to a 1 litre volumetric flask, dilute to the mark and mix well. Standardize this solution with a standard solution prepared from anhydrous sodium carbonate
27、. NOTE 1 0,053 5 g of ammonium chloride. 1 ml of 0.5 mol/i sulfuric acid is equivalent to 4.4 Sulfuric acid, 50 % (V/v) solution. Adopting appropriate safety precautions, carefully add 500 mi of sulfuric acid (Q = 1,84 g/ml) to 500 ml of water. Mix well. WARNING - This is a potentially dangerous pro
28、- cedure and should be carried out by a trained person. 4.5 Sodium hydroxide solution, 1 O mol/l. Dissolve 400 g of sodium hydroxide in water. Dilute to 1 litre and mix well. This solution should be pre- pared in a water-cooled polyethylene beaker and stored in a polyethylene bottle. CEN ENSISO 9455
29、-9 95 3404589 OLL9L38 T50 Page 4 EN IS0 9455-9 1995 4.6 Methyl orange indicator solution, 0,l g/100 ml. Dissclve ,1 g of methyl orange in 100 ml water. Mix well. 5 Apparatus in addition to ordinary laboratory apparatus, the appa- ratus shown in figure 1 is required. 6 Procedure Carry out the followi
30、ng procedure in triplicate on the flux sample. 6.1 Preparation of flux test solution 6.1.1 Solid fluxes Weigh 10 g of the solid flux sample into a 400 ml beaker. Add water and sufficient sulfuric acid solution (4.4) to clear the solution. Transfer to a 500 ml volumetric flask, dilute to the mark and
31、 mix. 6.1.2 Paste fluxes For water-soluble paste fluxes, weigh 10 g of the paste flux sample into a 400 ml beaker. Add water and sufficient sulfuric acid solution (4.4) to clear the solution. Transfer to a 500 ml volumetric flask, dilute to the mark and mix. NOTE 2 For non-water-soluble paste fluxes
32、, the method of preparation of the flux test solution can require modifi- cation. In such cases, advice should be sought from the manufacturer . 6.1.3 Liquid fluxes By means of a pipette, transfer 25 ml of the liquid flux sample to a 500 ml volumetric flask. Dilute to the mark and mix. Dropping funn
33、el Water-cooled condenser Distillation Receiver flask Figure 1 - Apparatus for determination of ammonia content CEN EN*ISO 9455-9 95 m 3404589 OLL9L39 997 m Page 5 EN IS0 9455-9 : 1995 Parameter Within laboratory: standard deviation s,., repeatability r Between laboratories standard deviation s, rep
34、roducibility R 6.2 Determinations Nominal ammonia content of test flux 2,3 % 7,O % 0,04 0,13 0.13 0,36 0.11 0.93 0.30 2.62 Set up the apparatus as shown in figure 1. Ensure that the open end of the water-cooled condenser is well below the level of the solution contained in the re- ceiver. By means o
35、f a pipette or burette, transfer 15,0 ml of the sulfuric acid solution (4.3) and 100 ml of water to the receiver. Transfer 100 ml of the flux test solution (6.1) to the distillation flask. Introduce 30 ml of the 10 moll1 sodium hydroxide solution (4.5) to the dropping fun- nel, with the tap closed.
36、Open the tap of the dropping funnel and run all but approximately 2 mi of the sodium hydroxide solution contained in the funnel into the flask. Heat the con- tents of the flask to boiling and boil briskly for 10 min, so that the ammonia present in the flux test solution is driven off and collected i
37、n the receiver. NOTE 3 Dortion of the sulfuric acid contained in the receiver. This ammonia reacts quantitatively with a pro- Wash the inside of the water-cooled condenser twice with water and add the washings to the receiver. Titrate the solution in the receiver with 1 mol/l sodium hydroxide soluti
38、on (4.21, using methyl orange (4.6) as indicator. 7 Calculation of results 7.1 Solid or paste flux samples The content of ammonia, w, expressed as a percent- age by mass cf ammonium chloride, is calculated for solid or paste flux samples, from the following for- mula: (15-V) x 0,053 5 x 5 lx w= rn w
39、hich can be simplified to 26,75 (1 5 - V) rn W= where V is the volume, in millilitres, of sodium hy- droxide solution (4.2) used in the titration; rn is the mass, in grams, of the solid or paste flux sample taken. 7.2 Liquid flux samples The content of ammonia, w, expressed as a percent- age by mass
40、 of ammonium chloride, is calculated for liquid flux samples from the following formula: 26,75 (1 5 - V) W= 25e where e is the density, in g/ml, of the liquid flux sample, at 20 “C. determined with a hydrometer. 8 Precision 8.1 General This method was subjected to a limited interlaboratory test prog
41、ramme. The repeatability and reproducibility of the method were calculated in accordance with IS0 5725” ; the results are given in 8.2. 8.2 Precision data Tests were carried out on two zinc chloride fluxes, containing nominal ammonia contents of 2,3 % and 7,O % respectively. Five laboratories took p
42、ari in the tests with the following results: 1 IS0 5725:1986, Precision of test methods - Determination of repeatability and reproducibility for a standard rest method by inter-laboratory tesrs CEN ENSISO 9455-9 95 = 3404589 OLLSL40 609 9 Page 6 EN IS0 9455-9 : 1995 9 Test report c) the results obta
43、ined; The test report shall include the following information: a) the identification of the test sample; b) the test method used (.e. reference of this part of IS0 9455); d) any unusual features noted during the determi- e) details of any operation not included in this part nation; of IS0 9455, or r
44、egarded as optional. - CEN ENxISO 9455-9 95 3404587 OLL7L4L 545 9 Page 7 EN IS0 9455-9 : 1995 Annex ZA (normative) Normative references to international publications with their relevant European publications “his European Standard incorporates by dated or undated reference, provisions from other pub
45、lications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revis
46、ion. For undated references the latest edition of the publication reerred to applies (including amendments). Publication Year Title EN/HD Year IS0 9454-1 1990 Safi solderng$uxes - Chfkation and EN 29454-1 1993 requirements - Part 1 : ClassQ%ation, labelling and packaging Q BSI 1996 BS EN IS0 9456-9
47、: 1996 List of references See national foreword. O BSI 1996 BS EN IS0 9455-9 : 1996 BSI 389 Chiswick High Road London w4 4AL BSI - British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the
48、 international level. It is incorporated by Royal Charter. Contract requirements A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Revisions British Standards are updated by amendment o
49、r revision. Users of British Standards should make sure that they possess the latest amendments or editions. Any person who finds an inaccuracy or ambiguity while using this British Standard should bring it to the attention of the Quality Manager, BSI without delay so that the matter may be investigated swiftly. BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of standards. Buying standards Orders for all BSI, international an
