1、BRITISH STANDARD BS EN ISO 9455-9:1996 Soft soldering fluxes Test methods Part 9: Determination of ammonia content The European Standard EN ISO9455-9:1995 has the status of a BritishStandard ICS 25.160.20;25.160.50BSENISO9455-9:1996 This BritishStandard, having been prepared under the directionof th
2、e Engineering SectorBoard, was published underthe authority of the Standards Board and comesintoeffect on 15February1996 BSI 01-2000 The following BSI references relate to the work on this standard: Committee reference NFE/27 Draft for comment92/42775DC ISBN 0 580 25230 2 Committees responsible for
3、this BritishStandard The preparation of this BritishStandard was entrusted to Technical Committee NFE/27, Tin and tin alloys, upon which the following bodies were represented: Association of British Pewter Craftsmen British Iron and Steel Producers Association Federation of the Electronics Industry
4、International Tin Research Institute London Metal Exchange Metal Packaging Manufacturers Association Solder Makers Association Co-opted members The following bodies were also represented in the drafting of the standard, through subcommittees and panels: British Plumbing Fittings Manufacturers Associ
5、ation Institute of Metal Finishing Ministry of Defence Co-opted members Amendments issued since publication Amd. No. Date CommentsBSENISO9455-9:1996 BSI 01-2000 i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 1 Scope 3 2 Normative reference 3 3 Principle 3 4
6、 Reagents 3 5 Apparatus 3 6 Procedure 3 7 Calculation of results 4 8 Precision 5 9 Test report 5 Annex ZA (normative) Normative references to international publicationswiththeir relevant European publications 6 Figure 1 Apparatus for determination of ammonia content 4 Table 1 5 List of references In
7、side back coverBSENISO9455-9:1996 ii BSI 01-2000 National foreword This British Standard has been prepared by Technical Committee NFE/27 and is the English language version of EN ISO9455-9:1995 Soft soldering fluxes Test methods Part9: Determination of ammonia content, published by the European Comm
8、ittee for Standardization (CEN). EN ISO9455-9:1995 is identical with ISO9455-9:1993, published by the International Organization for Standardization (ISO). A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their
9、correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-reference Publication referred to Corresponding BritishStandard ISO9454-1:1990 BS EN29454 Soft soldering fluxes. Classification and requirements Part1:1994 Classification, labelli
10、ng and packaging Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, theENISO title page, pages2 to6, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated i
11、n the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO9455-9 September1995 ICS 25.160.20;25.160.50 Descriptors: Soldering, soldering fluxes, tests, chemical analysis, determination of content, ammonia (gas), volumetric analysis English version Soft s
12、oldering fluxes Test methods Part9:Determination of ammonia content (ISO9455-9:1993) Flux de brasage tendre Mthodes dessai Partie9: Dosage de lammoniac (ISO9455-9:1993) Flu“mittel zum Weichlten Prfverfahren Teil9: Bestimmung des Ammoniumgehaltes (ISO9455-9:1993) This European Standard was approved b
13、y CEN on1995-08-27. 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 lists and bibliographical references concerning such national standards
14、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 to the C
15、entral 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 andUnitedKingdom. CEN European
16、 Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1995 All rights of reproduction and communication in any form and by any means reserved in all countries to CEN and its members. Ref. No. EN ISO9455-9
17、:1995 EENISO9455-9:1995 2 BSI 01-2000 Foreword The text of the International Standard from ISO/TC44, Welding and allied processes, of the International Organization for Standardization (ISO) has been taken over as a European Standard by the Technical Committee CEN/TC121, Welding. This European Stand
18、ard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by March1996, and conflicting national standards shall be withdrawn at the latest by March1996. According to the CEN/CENELEC Internal Regulations, the following countries
19、 are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, UnitedKingdom. NOTENormative references to International Standards are listed in Annex ZA (norm
20、ative).ENISO9455-9:1995 BSI 01-2000 3 1 Scope This part of ISO9455 specifies a distillation method for the determination of the ammonia content of solid, paste or liquid fluxes. The method is applicable to fluxes of class3.1.1 only, as defined in ISO9454-1. 2 Normative reference The following standa
21、rd contains provisions which, through reference in this text, constitute provisions of this part of ISO9455. 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 ISO9455 are encouraged to investigate the p
22、ossibility of applying the most recent edition of the standard indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO9454-1:1990, Soft soldering fluxes Classification and requirements Part1:Classification, labelling and packaging. 3 Principle The p
23、repared flux solution is distilled with sodium hydroxide 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
24、4.1 General Use only reagents of recognized analytical quality and only distilled, or deionized, water. 4.2 Sodium hydroxide solution, 1,0 mol/l standard solution, commercially available. Alternatively, use an approximately1,0mol/l solution of sodium hydroxide, prepared by the following method. Diss
25、olve40g of sodium hydroxide in water and cool. Transfer the solution to a1litre volumetric flask, dilute to the mark and mix well. Standardize this solution with0,5mol/l sulfuric acid solution(4.3). 4.3 Sulfuric acid, 0,5mol/l, standard solution, commercially available. Alternatively, use an approxi
26、mately0,5mol/l solution of sulfuric acid prepared by the following method. Cautiously add30ml of sulfuric acid( =1,84g/ml) to400ml of water and mix. Cool and transfer to a1litre volumetric flask, dilute to the mark and mix well. Standardize this solution with a standard solution prepared from anhydr
27、ous sodium carbonate. NOTE 11ml of0,5mol/l sulfuric acid is equivalent to0,0535g of ammonium chloride. 4.4 Sulfuric acid, 50% (V/V) solution. Adopting appropriate safety precautions, carefully add500ml of sulfuric acid( =1,84g/ml) to500ml of water. Mix well. WARNING This is a potentially dangerous p
28、rocedure and should be carried out by a trained person. 4.5 Sodium hydroxide solution, 10mol/l. Dissolve400g of sodium hydroxide in water. Dilute to1litre and mix well. This solution should be prepared in a water-cooled polyethylene beaker and stored in a polyethylene bottle. 4.6 Methyl orange indic
29、ator solution, 0,1g/100ml. Dissolve0,1g of methyl orange in100ml water. Mix well. 5 Apparatus In addition to ordinary laboratory apparatus, the apparatus shown in Figure 1 is required. 6 Procedure Carry out the following procedure in triplicate on the flux sample. 6.1 Preparation of flux test soluti
30、on 6.1.1 Solid fluxes Weigh10g of the solid flux sample into a400ml beaker. Add water and sufficient sulfuric acid solution(4.4) to clear the solution. Transfer to a500ml volumetric flask, dilute to the mark and mix. 6.1.2 Paste fluxes For water-soluble paste fluxes, weigh10g of the paste flux sampl
31、e into a400ml beaker. Add water and sufficient sulfuric acid solution(4.4) to clear the solution. Transfer to a500ml volumetric flask, dilute to the mark and mix. NOTE 2For non-water-soluble paste fluxes, the method of preparation of the flux test solution can require modification. In such cases, ad
32、vice should be sought from the manufacturer. 6.1.3 Liquid fluxes By means of a pipette, transfer25ml of the liquid flux sample to a500ml volumetric flask. Dilute to the mark and mix. ENISO9455-9:1995 4 BSI 01-2000 6.2 Determinations Set up the apparatus as shown in Figure 1. Ensure that the open end
33、 of the water-cooled condenser is well below the level of the solution contained in the receiver. By means of a pipette or burette, transfer15,0ml of the sulfuric acid solution(4.3) and100ml of water to the receiver. Transfer100ml of the flux test solution(6.1) to the distillation flask. Introduce30
34、ml of the10mol/l sodium hydroxide solution(4.5) to the dropping funnel, with the tap closed. Open the tap of the dropping funnel and run all but approximately2ml of the sodium hydroxide solution contained in the funnel into the flask. Heat the contents of the flask to boiling and boil briskly for10m
35、in, so that the ammonia present in the flux test solution is driven off and collected in the receiver. NOTE 3This ammonia reacts quantitatively with a proportion of the sulfuric acid contained in the receiver. Wash the inside of the water-cooled condenser twice with water and add the washings to the
36、 receiver. Titrate the solution in the receiver with1mol/l sodium hydroxide solution(4.2), 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 percentage by mass of ammonium chloride, is calculated for solid or pas
37、te flux samples, from the following formula: which can be simplified to Figure 1 Apparatus for determination of ammonia content where V is the volume, in millilitres, of sodium hydroxide solution(4.2) used in the titration; m is the mass, in grams, of the solid or paste flux sample taken.ENISO9455-9
38、:1995 BSI 01-2000 5 7.2 Liquid flux samples The content of ammonia, w, expressed as a percentage by mass of ammonium chloride, is calculated for liquid flux samples from the following formula: where is the density, ing/ml, of the liquid flux sample, at20 C, determined with a hydrometer. 8 Precision
39、8.1 General This method was subjected to a limited interlaboratory test programme. The repeatability and reproducibility of the method were calculated in accordance with ISO5725 1) ; the results are given in8.2. 8.2 Precision data Tests were carried out on two zinc chloride fluxes, containing nomina
40、l ammonia contents of2,3% and7,0% respectively. Five laboratories took part in the tests with the following results: Table 1 9 Test report The test report shall include the following information: a) the identification of the test sample; b) the test method used (i.e.reference of this part of ISO9455
41、); c) the results obtained; d) any unusual features noted during the determination; e) details of any operation not included in this part of ISO9455, or regarded as optional. 1) ISO5725:1986, Precision of test methods Determination of repeatability and reproducibility for a standard test method by i
42、nter-laboratory tests Parameter Nominal ammonia content of test flux 2,3% 7,0% Within laboratory: standard deviation repeatability s w r 0,04 0,13 0,13 0,36 Between laboratories standard deviation reproducibility s b R 0,11 0,30 0,93 2,62ENISO9455-9:1995 6 BSI 01-2000 Annex ZA (normative) Normative
43、references to international publications with their relevant European publications This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereaft
44、er. 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 revision. For undated references the latest edition of the publication referred to applies (including amendments). Publication Yea
45、r Title EN/HD Year ISO9454-1 1990 Soft soldering fluxes Classification and requirements Part1: Classification, labelling and packaging EN29454-1 1993BSENISO9455-9:1996 BSI 01-2000 List of references See national foreword.BS EN ISO 9455-9:1996 BSI 389 Chiswick High Road London W4 4AL BSIBritishStanda
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