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1、INTERNATIONAL STANDARD IS0 9455-6 First edition 1995-09-I 5 Soft soldering fluxes - Test methods - Part 6: Determination and detection of halide (excluding fluoride) content Flux de brasage tendre - Mkthodes dessai - Partie 6: Dosage et detection des halogkwres (21 /exception des fluorures) Referenc
2、e number IS0 9455-6:1995(E) Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 20:52:12 MDTNo reproduction or networking permitted without license from IHS -,-,- Foreword IS0 (the i
3、nternational Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member body interested in a subject for which a technical committee
4、has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnica
5、l standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard IS0 9455-6 was prepared by Tech
6、nical Committee ISO/TC 44, We/ding and allied processes, Subcommittee SC 12, Soldering and brazing materials. IS0 9455 consists of the following parts, under the general title Soft soldering fluxes - Test methods: - Part 1: Determination of non-volatile matter, gravimetric method - Part 2: Determina
7、tion of non-volatile matter, ebulliometric method - Part 3: Determination of acid value, potentiometric and visual titration methods - Part 5: Copper mirror test - Part 6: Determination and detection of halide (excluding fluoride) content - Part 8: Determination of zinc content - Part 9: Determinati
8、on of ammonia content - Part 10: Flux efficacy tests, solder spread method - Part 11: Solubility of flux residues 0 IS0 1995 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized In any form or by any means, electronic or mechanical, including pho
9、tocopyrng and mrcrofilm, wrthout permrssron In wrttrng from the publisher. lnternatronal Organizatron for Standardization Case Postale 56 ? CH-1211 Geneve 20 ? Switzerland Printed In Switzerland ii Copyright International Organization for Standardization Provided by IHS under license with ISO Licens
10、ee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 20:52:12 MDTNo reproduction or networking permitted without license from IHS -,-,- Q IS0 IS0 9455-6:1995(E) - Part 12: Steel tube corrosion test - Part 13: Determination of flux spattering - Part 14: Assessment of tackiness of flux
11、residues - Part 15: Copper corrosion test - Part 16: Flux efficacy tests, wetting balance method T.echnical Report - Part 17: Determination of surface insulation resistance of flux resi- dues (Comb test) - Part 18: Electrochemical migration test for flux residues Annex A forms an integral part of th
12、is part of IS0 9455. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 20:52:12 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD 0 I
13、S0 IS0 9455-6:1995(E) Soft soldering fluxes - Test methods - Part 6: Determination and detection of halide (excluding fluoride) content 1 Scope This part of IS0 9455 specifies three quantitative methods for the determination of the ionic halide (ex- cluding fluoride) content of soldering fluxes. Hal
14、ides are calculated as chlorides. A useful qualitative test method for the detection of ionic halides is also de- scribed. Method A is a potentiometric titration method for the determination of halide (excluding fluoride) content and is applicable to flux classes 1 and 2, defined in IS0 9454-l. This
15、 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 the flux. Method B is a titration method for the determination of the total halide (excluding fluoride) content
16、 of water-soluble fluxes. It is applicable to flux classes 2.1.2.A and 3.1 .l .A, as defined in IS0 9454-l. Method C is a titration method for the determination of the halide (excluding fluoride) content of water- soluble fluxes containing phosphates and is applica- ble to flux class 3.2.1 .A, as de
17、fined in IS0 9454-l. 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 references The following standards contain provisions which, through reference in this text, constitute provisions
18、of this part of IS0 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 IS0 9455 are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below
19、. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 5725-2: 1994, Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method. IS0 9454-
20、l :I 990, Soft soldering fluxes - Classifi- cation and requirements - Part 1: Classification, labelling and packaging. IS0 9455-l :I 990, Soft soldering fluxes - Test meth- ods - Part 1: Determination of non-volatile matter, gravimetric method. IS0 9455-2: 1993, Soft soldering fluxes - Test meth- od
21、s - 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 resulting solution is titrated with standard silver nitrate solution, using a silv
22、er electrode, the mV readings being recorded simul- 1 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 20:52:12 MDTNo reproduction or networking permitted without license from IHS
23、 -,-,- IS0 9455-6:1995(E) 0 IS0 taneously. From the graph of volume of titrant readings against mV readings, the point of inflexion is determined and the percentage halide content, ex- pressed as chloride, is calculated. The method is not suitable for the determination of fluoride. This method is ap
24、plicable to flux classes 1 and 2, as defined in IS0 9454-l. 3.2 Reagents 3.2.1 General Only reagents of recognized analytical quality and distilled or deionized water with a conductivity less than 10 j and b) for flux samples having a halide ion concentration in the range 1 % (m/m) to 2 % (m/m), the
25、 mass of sample taken should be halved. Add 100 ml of propan-2-01 (3.2.21, or water, according to the solubility characteristics of the flux (see note 4). Cover with a watch glass and allow to dis- solve with gentle agitation. NOTE 4 For fluxes of class 1.2, as defined in IS0 9454-l the choice of so
26、lvent should be agreed between the flux manufacturer and the user. Place the beaker on the stand of the titration as- sembly with the electrodes, stirrer and burette in position. Adjust the speed of the stirrer to give vigor- ous stirring without splashing. Titrate with the silver nitrate solution (
27、3.2.31, adding 1 ml portions and re- cording the mV meter readings after each addition. As the end-point is approached, reduce the additions of titrant to 0,l ml and continue titrating past the end-point. Plot the potential values against the volume of titrant added to obtain the titration curve. Th
28、e point of in- flexion of the curve corresponds to the end-point of the titration. NOTE 5 The point of inflexion of the curve may con- veniently be determined by using the derivative curve. Carry out a blank determination, using all reagents, for comparison purposes. Copyright International Organiza
29、tion for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 20:52:12 MDTNo reproduction or networking permitted without license from IHS -,-,- 0 IS0 3.5 Calculation of results The halide (excluding fluoride) content, expre
30、ssed as the percentage, by mass, of chloride in the flux, is given by: 0,070 9 x v m fl where V is the volume, in millilitres, of silver nitrate solution used, less the volume needed to titrate the blank; f, is the correlation factor for the silver nitrate solution (see 3.2.3); m is the mass, in gra
31、ms, of the sample taken. The halide content of the flux sample is given by the mean of the three results obtained on the triplicate test samples. The halide content may also be expressed as the percentage, by mass, of chloride in the non-volatile matter by: 7,09 x v mS fl where s is the percentage n
32、on-volatile matter con- tent of the sample, determined as de- scribed in IS0 9455-l or IS0 9455-2. For solid flux samples, S = 100. 4 Method B: Titration method for halide (excluding fluoride) content of water- soluble fluxes 4.1 Principle A prepared sample of the flux is diluted to a known volume w
33、ith water and a specified volume of sulfuric acid of known concentration. The solution IS then treated with a known quantity of silver nitrate solution and the excess silver nitrate is titrated with am- monium thiocyanate. A blank determination using water in place of the flux is carried out simulta
34、neously and the percentage halide content, expressed as chloride, is calculated. The method is not suitable for the determination of fluoride. The test is applicable to fluxes of classes 2.1.2.A and IS0 9455-6:1995(E) 3.1 .I .A only, as defined in IS0 9454-l. Some liquid fluxes contain free hydrochl
35、oric acid and the halide content will, consequently, be greater than the amount equivalent to the zinc and other chlorides present. 4.2 Reagents 4.2.1 General Only reagents of recognized analytical quality and distilled or deionized water with a conductivity less than 10 pS/cm are to be used. 4.2.2
36、Silver nitrate solution (0.1 mol/l). 16,99 g of silver nitrate (AgNO,) are dissolved in water (see note 1) then transferred to a 1 litre volu- metric flask and diluted to the mark with water. This is mixed thoroughly. Alternatively, a commercially available concentrate is used to prepare 0,l mol/l s
37、tandard silver nitrate sol- ution. The silver nitrate solution is standardized using the method given in annex A, to derive the correlation factorf,. This is stored in an amber glass bottle. NOTES 6 The silver nitrate (AgNO,) should be dried at 110 “C f 5 “C for 16 h and cooled in a desiccator befor
38、e weighing. 7 1 ml of silver nitrate solution (4.2.2) is equivalent to 0,003 545 xf2 grams of chloride ion. 4.2.3 Ammonium thiocyanate solution (approxi- mately 0,l mol/l). 8 g of ammonium thiocyanate (NH,CNS) are dissolved in water then transferred to a 1 litre volumetric flask and diluted to the m
39、ark with water. This is mixed thoroughly. Alternatively, a commercially available concentrate is used to prepare 0,l mol/l standard ammonium thio- cyanate solution. 4.2.4 Sulfuric acid solution 20 % (V/V). 200 ml of sulfuric acid (density I,84 g/ml) is cautiously added, with stirring, to 400 ml of w
40、ater. It is then mixed, cooled, diluted to 1 litre and mixed thoroughly. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 20:52:12 MDTNo reproduction or networking permitted witho
41、ut license from IHS -,-,- IS0 9455-6:1995(E) Q IS0 4.2.5 Ammonium ferric sulfate indicator solution. 10 g of ammonium ferric sulfate NH,Fe(SO,),.12H,O are dissolved in 100 ml water. 4.2.6 Nitrobenzene WARNING - Care should be exercised in the handling and disposal of this hazardous reagent. 4.2.7 Ni
42、tric acid (density I,42 g/ml). 4.3 Apparatus Ordinary laboratory apparatus. 4.4 Procedure Carry out the following procedure, in triplicate, on the flux sample. By means of a pipette, transfer 25 ml of the sample to a 500 ml volumetric flask. Add 10 ml of sulfuric acid solution (4.2.41, dilute to the
43、 mark with water and mix. By means of a pipette, transfer 10 ml of this solution to a glass-stoppered 500 ml conical flask and add 50 ml of water, followed bv 5 ml of nitric acid (4.2.7). To a similar flask transfer 60 ml of water and 5 ml of nitric acid (4.2.7) and carry out, simultaneously, a blan
44、k determination following the same procedure and using the same quantities of reagents as used for the flux sample. By means of a burette or a pipette, add 50 ml of silver nitrate solution (4.2.2) to the contents of the flask. NOTE 8 2 ml of nitrobenzene (4.2.6) may be added to assist coagulation of
45、 the precipitate. Re-stopper the flask and shake it vigorously. Add 5 ml of ammonium ferric sulfate indicator solution (4.2.5) and titrate with ammonium thiocyanate sol- ution (4.2.31, shaking the flask vigorously between additions of the titrant. The end-point is indicated when a faint orange-red c
46、olour first persists through- out the solution in the flask. 4.5 Standardization of the ammonium thiocyanate solution (4.2.3) Transfer 70 ml of water and 5 ml of nitric acid (4.2.7) to a 500 ml conical flask. By means of a pipette, add 25 ml of silver nitrate solution (4.2.2). Add 5 ml of ammonium f
47、erric sulfate indicator solution (4.2.5) and titrate with the ammonium thiocyanate solution (4.2.31, as in the procedure given in 4.4. Calculate the correlation factor f3 for the ammonium thiocyanate, as follows: i3= 25 xf2 volume of NH,CNS 4.6 Calculation of results The halide (excluding fluoride)
48、content, expressed as the percentage by mass of chloride in the flux, is given by the following formula: (titreblank - titre sample) x 0,003 545 x.h 0,5 d 1 x 1oo which simplifies to: 0,709 x v d f3 where: V is the volume, in millilitres, of ammonium thiocyanate solution (4.2.3) used in the titratio
49、n of the blank, minus the volume used in the titration of the flux sample; d is the density, in grams per millilitre, of the original flux sample, at 20 “C, determined by the use of a hydrometer; f3 is the correlation factor for the ammonium thiocyanate obtained in 4.5. The halide content of the flux sample is given by the mea