1、BRITISH STANDARD BS EN ISO 9455-6:1997 Soft soldering fluxes Test methods Part 6: Determination and detection of halide (excluding fluoride) content The European Standard EN ISO 9455-6:1997 has the status of a British Standard ICS 25.160.50BSEN ISO 9455-6:1997 This British Standard, having been prep
2、ared under the direction of the Engineering Sector Board, was published under the authority of the Standards Board and comes into effect on 15 April 1997 BSI 11-1998 ISBN 0 580 26522 6 National foreword This British Standard is the English language version of EN ISO 9455-6:1997. It is identical with
3、 ISO 9455-6:1995. It partially supersedes BS 5625:1985 which will be withdrawn following publication of other European standards in this series. The UK participation in its preparation was entrusted by Technical Committee NFE/27, Tin and tin alloys, to Subcommittee NFE/27/4, Solders and soldering fl
4、uxes, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promu
5、lgate them in the UK. A list of organizations represented on this committee can be obtained on request. Cross-references Attention is drawn to the fact that annex ZA lists normative references to international publications with their corresponding European publications. The British Standards which i
6、mplement these international or European publications may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the
7、necessary provisions of a contract. Users of British Standards are responsible for their correct 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, pages i and ii, t
8、heENtitlepage, page 2, the ISO title page, pages ii to iv, pages 1 to 10 andaback cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No.
9、 Date CommentsBSEN ISO 9455-6:1997 BSI 11-1998 i Contents Page National Foreword Inside front cover Foreword 2 Text of ISO 9455-6 1 ii blankEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 9455-6 January 1997 ICS 25.160.50 Descriptors: See ISO document English version Soft soldering fluxes T
10、est methods Part6:Determination and detection of halide (excludingfluoride) content (ISO 9455-6:1995) Flux de brasage tendre Mthodes dessai Partie 6: Dosage et dtection des halognures ( lexception des fluorures) (ISO 9455-6:1995) Flumittel zum Weichlten Prfverfahren Teil 6: Bestimmung und Nachweis d
11、es Halogenidgehaltes (auer Fluorid) (ISO 9455-6:1995) This European Standard was approved by CEN on 1996-12-12. 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 alt
12、eration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. The European Standards exist in three official versions (English, French, German). A version in any other language made by trans
13、lation under the responsibility 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, Luxembour
14、g, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart, 36 B-1050 Brussels 1997 Copyright reserved to CEN members Ref. No. EN ISO 94
15、55-6:1997 EENISO 9455-6:1997 BSI 11-1998 2 Foreword The text of the International Standard from Technical Committee ISO/TC 44 “Welding and allied processes” of the International Organization for Standardization (ISO) has been taken over as an European Standard by Technical Committee CEN/TC 121 “Weld
16、ing”, the secretariat of which is held byDS. 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 July 1997, and conflicting national standards shall be withdrawn at the latest by July 1997. According
17、to the CEN/CENELEC Internal Regulations, the national standards organizations of 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, Swit
18、zerland and the United Kingdom. Endorsement notice The text of the International Standard ISO9455-6:1995 has been approved by CEN as a European Standard without any modification. NOTENormative references to International Standards are listed in annex ZA (normative).ENISO 9455-6:1997 ii BSI 11-1998 C
19、ontents Page Foreword iii 1 Scope 1 2 Normative references 1 3 Method A: Potentiometric method 1 3.1 Principle 1 3.2 Reagents 1 3.3 Apparatus 1 3.4 Procedure 1 3.5 Calculation of result 2 4 Method B: Titration method for halide (excluding fluoride) content of water-soluble fluxes 2 4.1 Principle 2 4
20、.2 Reagents 2 4.3 Apparatus 3 4.4 Procedure 3 4.5 Standardization of the ammonium thiocyanate solution (4.2.3) 3 4.6 Calculation of results 3 5 Method C:Titration method for the determination of halide (excluding fluoride) content of water-soluble fluxes containing phosphates 4 5.1 Principle 4 5.2 R
21、eagents 4 5.3 Apparatus 4 5.4 Procedure 4 5.5 Standardization of the ammonium thiocyanate solution (5.2.3) 4 5.6 Calculation of results 5 6 Method D: Qualitative test for the presence of ionic halides in flux 5 6.1 Principle 5 6.2 Reagents 5 6.3 Apparatus 5 6.4 Procedure 5 7 Precision 6 7.1 General
22、6 7.2 Method A 6 7.3 Method B 6 7.4 Method C 6 8 Test report 7 Annex A 8 Annex ZA 10ENISO 9455-6:1997 BSI 11-1998 iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Stan
23、dards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also t
24、ake part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an Internationa
25、l Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard ISO 9455-6 was prepared by Technical Committee ISO/TC 44, Welding and allied processes, Subcommittee SC 12, Soldering and brazing materials. ISO 9455 consists of the following parts, under the g
26、eneral title Soft soldering fluxes Test methods: Part 1: Determination of non-volatile matter, gravimetric method; Part 2: Determination of non-volatile matter, ebulliometric method; Part 3: Determination of acid value, potentiometric and visual titration methods; Part 5: Copper mirror test; Part 6:
27、 Determination and detection of halide (excluding fluoride) content; Part 8: Determination of zinc content; Part 9: Determination of ammonia content; Part 10: Flux efficacy tests, solder spread method; Part 11: Solubility of flux residues; Part 12: Steel tube corrosion test; Part 13: Determination o
28、f flux spattering; Part 14: Assessment of tackiness of flux residues; Part 15: Copper corrosion test; Part 16: Flux efficacy tests, wetting balance method Technical Report; Part 17: Determination of surface insulation resistance of flux residues (Comb test); Part 18: Electrochemical migration test f
29、or flux residues. Annex A forms an integral part of this part of ISO 9455. Descriptors: Soldering, soldering fluxes, tests, chemical analysis, detection, determination of content, halides, volumetric analysis.iv blankBSEN ISO 9455-6:1997 BSI 11-1998 1 1 Scope This part of ISO 9455 specifies three qu
30、antitative methods for the determination of the ionic halide (excluding fluoride) content of soldering fluxes. Halides are calculated as chlorides. A useful qualitative test method for the detection of ionic halides is also described. Method A is a potentiometric titration method for the determinati
31、on of halide (excluding fluoride) content and is applicable to flux classes 1 and 2, defined in ISO 9454-1. This method, which is to be considered the reference method for these fluxes, is suitable for halide contents generally within the range 0,05 % (m/m) to 2 % (m/m) in the non-volatile matter of
32、 the flux. Method B is a titration method for the determination of the total halide (excluding fluoride) content of water-soluble fluxes. It is applicable to flux classes 2.1.2.A and 3.1.1.A, as defined in ISO 9454-1. Method C is a titration method for the determination of the halide (excluding fluo
33、ride) content of water-soluble fluxes containing phosphates and is applicable to flux class 3.2.1.A, as defined in ISO 9454-1. Method D is a qualitative test, using silver chromate test paper, for the presence of ionic halides. The technique may be used for all classes of flux. 2 Normative reference
34、s The following standards contain provisions which, through reference in this text, constitute provisions of this part of ISO 9455. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this part of ISO 9455 are encou
35、raged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method
36、 for the determination of repeatability and reproducibility of a standard measurement method. ISO9454-1:1990, Soft soldering fluxes Classification and requirements Part1:Classification, labelling and packaging. ISO9455-1:1990, Soft soldering fluxes Test methods Part 1: Determination of non-volatile
37、matter, gravimetric method. ISO9455-2:1993, Soft soldering fluxes Test methods Part 2: Determination of non-volatile matter, ebulliometric method. 3 Method A: Potentiometric method (Reference method) 3.1 Principle A prepared, weighed sample of the flux is dissolved in a suitable solvent. The resulti
38、ng solution is titrated with standard silver nitrate solution, using a silver electrode, the mV readings being recorded simultaneously. From the graph of volume of titrant readings against mV readings, the point of inflexion is determined and the percentage halide content, expressed as chloride, is
39、calculated. The method is not suitable for the determination of fluoride. This method is applicable to flux classes 1 and 2, as defined in ISO 9454-1. 3.2 Reagents 3.2.1 General Only reagents of recognized analytical quality and distilled or deionized water with a conductivity less than 10 S/cm are
40、to be used. 3.2.2 Propan-2-ol 3.2.3 Silver nitrate solution (0,02 mol/l) 3,4 g of silver nitrate (AgNO 3 ) are dissolved in water (see note 1) then transferred to a 1 litre volumetric flask and diluted to the mark with water. It is mixed thoroughly. Alternatively a commercially available concentrate
41、 is used to prepare 0,02 mol/l standard silver nitrate solution. The silver nitrate solution is standardized using the method given in annex A, to derive the correlation factor f 1 . This is stored in an amber glass bottle. NOTE 1The silver nitrate (AgNO 3 ) should be dried at110C 5 C for 16 h and c
42、ooled in a desiccator before weighing. NOTE 21 ml of silver nitrate solution (3.2.3) is equivalent to0,000 709 f 1g of chloride ion. 3.3 Apparatus Ordinary laboratory apparatus and 3.3.1 Millivolt meter 3.3.2 Silver electrode 3.3.3 Mercury/mercurous sulfate 1mol/l sodium sulfate electrode, or a reve
43、rsible hydrogen electrode. 3.3.4 Magnetic or mechanical stirrer, with variable speed drive, the stirrer bar to be PTFE-coated. 3.4 Procedure Carry out the following procedure, in triplicate, on the flux sample.BSEN ISO 9455-6:1997 2 BSI 11-1998 Weigh, to the nearest 0,001 g, approximately 0,5 g of t
44、he solid flux sample or 2 g of the liquid flux sample, avoiding loss of volatile matter during the weighing, and transfer it to a 250 ml low-form beaker. NOTE 3This procedure is suitable for halide ion concentrations generally within the range 0,1% (m/m) to 1% (m/m) in the non-volatile content of th
45、e solution to be titrated. For flux samples having halide ion concentrations outside this range, the sample mass taken should be adjusted, as follows: a) for flux samples having a halide ion concentration in the range 0,05 % (m/m) to 0,1 % (m/m), the mass of sample taken should be double; and b) for
46、 flux samples having a halide ion concentration in the range 1 % (m/m) to 2 % (m/m), the mass of sample taken should be halved. Add 100 ml of propan-2-ol (3.2.2), or water, according to the solubility characteristics of the flux (seenote 4). Cover with a watch glass and allow to dissolve with gentle
47、 agitation. NOTE 4For fluxes of class 1.2, as defined in ISO 9454-1 the choice of solvent should be agreed between the flux manufacturer and the user. Place the beaker on the stand of the titration assembly with the electrodes, stirrer and burette in position. Adjust the speed of the stirrer to give
48、 vigorous stirring without splashing. Titrate with the silver nitrate solution (3.2.3), adding 1 ml potions and recording the mV meter readings after each addition. As the end-point is approached, reduce the additions of titrant to 0,1 ml and continue titrating past the end-point. Plot the potential
49、 values against the volume of titrant added to obtain the titration curve. The point of inflexion of the curve corresponds to the end-point of the titration. NOTE 5The point of inflexion of the curve may conveniently be determined by using the derivative curve. Carry out a blank determination, using all reagents, for comparison purposes. 3.5 Calculation of results The halide (excluding fluoride) content, expressed as the percentage, by mass, of chloride in the flux, is given by: where
