ISO-9455-10-1998.pdf
STD-IS0 9955-1O-ENGL 1998 D 4851903 0755700 T72 INTERNATIONAL STANDARD IS0 9455-1 O First edition 1998-08-01 Soft soldering fluxes - Test methods - Part 1 O: Flux efficacy tests, solder spread method Flux de brasage tendre - Méthodes d'essai - Partie 10: Essais d'efficacité du flux, méthode d'étalement This material is reproduced from IS0 documents under Internattonai Organization for Standardization (ISO) Copyright License number IHSilCC11996. Not for resale. No part of these IS0 documents may be reproduced in any form, electronic retrieval system or otherwise, except as allowed in the copyright law of the country of use, or with the prior written consent of IS0 (Case postale 56,121 1 Geneva 20, Switzerland, Fax +41 22 734 10 79), IHS or the IS0 Licensor's members. Reference number IS0 9455-10:1998(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 21:44:30 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-IS0 7'i55-LO-ENGL 1978 Li851903 0755901 929 IS0 9455-1 O: 1998( E) Contents Page 1 Scope 1 2 Normative references . . 1 3 Principle 1 4 Reagents . 2 5 Apparatus . 2 6 Test specimens . . . . . . . . 3 7 Procedure . 3 8 Expression of results . . . . 4 9 Precision . 4 1 O Test report . . 5 Annex A (informative) Method for the preparation of standard reference rosin (colophony) based liquid fluxes, having 25 % (m/m) non-volatile content . 6 Annex B (informative) Chemical composition of brass test plates . . 8 Annex C (informative) Bibliography 9 O IS0 1998 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 photocopying and microfilm, without permission in writing from the publisher. International Organization for Standardization Case postale 56 CH-121 1 Genève 20 Switzerland Internet isoQiso.ch Printed in Switzerland Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 21:44:30 MDTNo reproduction or networking permitted without license from IHS -,-,- 8 IS0 Foreword IS0 (the International 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 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 electrotechnical 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. Intemational Standard IS0 9455-1 O was prepared by Technical Committee ISOíTC 44, Welding 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: 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: Determination and detection of halide (excluding fluoride) content - Part 8: Determination of zinc content - Pari 9: Determination of ammonia content - Part 1 O : Flux efficacy tests, solder spread method - Part 1 1: Solubility of flux residues - Part 12: Steel tube corrosion test - Part 13: Determination of flux spattering - Part 14: Assessment of tackiness of flux residues - Part 15: Copper corrosion test - Part 16: Flux efficacy tests, wetting balance method - Part 17: Surface insulation resistance, comb test and electrochemical migration test of flux residues Annexes A to C of this pari of IS0 9455 are for information only. . 111 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 21:44:30 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD o IS0 IS0 9455-1 0:1998(E) Soft soldering fluxes - Test methods - Part 1 O: Flux efficacy tests, solder spread method I scope This part of IS0 9455 specifies a method for the determination of the efficacy of a soft soldering flux. The method is known as the solder spread method and is applicable to all flux classes defined in IS0 9454-1, NOTES 1 This part of IS0 9455 is only applicable for liquid fluxes 10 % ( m h ) . 2 An alternative method for the determination of the flux efficacy, applicable to liquid fluxes only, known as the wetting balance method, is specified in IS0 9455-16. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions 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 edition of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 197-1 :1983, Copper and copper alloys - Terms and definitions - Part 1: Materials. IS0 1634-1 :1987, Wrought copper and copper alloy plate, sheet and strip - Part 1: Technical conditions of delivery for plate, sheet and strip for general purposes. IS0 361 1 :1978, Micrometer callipers for external measurement. IS0 9453:1990, Soft solder alloys - Chemical compositions and forms. IS0 9454-1 :1990, Soft soldering fluxes - Classification and requirements - Part 1: Classification, labelling and packaging. 3 Principle A specially prepared brass test sheet is treated with a known quantity of the flux under test and a standard quantity of specified solder alloy. Upon heating, the solder alloy melts and spreads across the surface of the brass test sheet, the extent of spread being a measure of the flux efficacy. The area covered by the solder is determined by means of a planimeter, or other suitable technique. This test method is applicable to all fluxes. If required, the efficacy of the flux sample under test can be compared with that of a standard flux (see annex A). NOTE - It is possible to use copper as the test surface. However, it is preferable to use brass as the test surface in order to distinguish between various fluxes because it provides a better surface for differentiation than copper would. 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 21:44:30 MDTNo reproduction or networking permitted without license from IHS -,-,- o IS0 4 Reagents Use only reagents of recognized analytical quality and only distilled or deionized water. 4.1 Acid preparation solution, prepared in a fume cupboard by cautiously mixing the following ingredients in the order given, cooling as necessary. - 140 ml water; - 225 ml nitric acid (p = 1,42 mi); - 600 ml sulphuric acid (p = 1,84 g/ml); - 5 g sodium chloride; - 18 ml copper solution (4.2). Thoroughly mix the solution. This preparation solution shall be freshly prepared every day. WARNING: The mixture is extremely corrosive and produces hazardous fumes. 4.2 Copper solution, prepared by dissolving 10 g pure copper (analytical grade) turnings in 100 ml of 50 % (Viv) nitric acid solution (p = 1,42 g/ml). 4.3 Industrial methylated spirits. 4.4 Acetone. 5 Apparatus 5.1 Solder bath, containing not less than 4 kg of molten tin-lead solder, having a liquidus of less than 200 OC. The liquid solder in the bath shall be at least 25 mm in depth, with a surface area easily capable of accommodating the test specimen. The bath shall be capable of being maintained at a temperature of 300 O C i 5 OC. 5.2 Tongs, or other suitable mechanical device, for lowering the brass test plate (6.1), in a horizontal plane, onto the surface of the liquid solder in the bath (5.1) and raising it again, also in a horizontal plane. 5.3 Planimeter, suitable for measuring surface areas of the order of 100 m d . 5.4 Microsyringe, or micropipette, capable of delivering 25 pl (¡.e. 0,025 mi). 5.5 Plastic tweezers or tongs, for use in the cleaning procedure for test plates. 5.6 Micrometer, as specified in IS0 361 1. 5.7 Filter paper, for use in cleaning procedure for test plates. 2 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 21:44:30 MDTNo reproduction or networking permitted without license from IHS -,-,- o IS0 STDmISO 9455-3O-ENGL 1998 D 4853903 0755905 57q m IS0 9455-1 Oz1 998(E) 6 Test specimens 6.1 Brass test plates Each plate shall be of 40 mm x 40 mm. Ten (10) plates cut from brass sheet, 0,5 mm thick, complying with IS0 1634-1 alloy CuZn37 or CuZn40, condition HA, for each flux being tested. NOTES 1 Annex B gives the chemical composition of these two brasses. 2 Copper test plates, each 40 mm x 40 mm. Ten (10) plates cut from phosphorus deoxidized sheet, 0,5 mm thick, complying with IS0 197-1, for each flux being tested, may also be used. 3 One corner of the test plate may be bent, to facilitate handling with the tongs (5.2). 6.2 Solder sample Clean a length of S-Sn6O Pb40 solder wire, with a diameter of 1 mm f 0,05 mm, weighing between 0,49 g and 0,50 g and complying with IS0 9453 with a filter paper soaked in industrial methylated spirits (4.3) or acetone (4.4). Wind the length of wire into a tight, flat spiral for use in the test. After cleaning, handle the solder wire only with clean cotton gloves. 7 Procedure 7.1 Preparation of test plates Immediately before use pretreat the ten test pieces in the following manner; handle with clean tongs or with a suitable mechanical device (5.2). Degrease the test plates (6.1) thoroughly in acetone (4.4) and allow to dry in clean air. Immerse each test plate separately for approximately 15 s, in the acid preparation solution (4.1) using the plastic tweezers or tongs (5.5). Hold the solution at a temperature between 15 O C and 25 OC. Wash the test plates in distilled or deionized water for a maximum of 5 s. Repeat the acid preparation operation, not more than three times, until a uniform matt lustre on the surface of the test plates has been attained. After the final rinsing in deionized water, rinse the test plates in methylated spirits (4.3) and dry them with filter paper (5.7). NOTE -This preparation method is applicable to both brass and copper test plates. 7.2 Test method Immediately after the cleaning operation described in 7.1, take one of the test plates and apply the flux sample under test to the central region of the plate, in accordance with a) or b) as follows: a) For liquid flux samples: measure 0,025 ml * 5 % of the sample by means of the microsyringe or micropipette (5.4); b) For paste flux samples: weigh 0,025 g * 5 % of the sample. Place a solder sample (6.2) in the middle of the test plate. Lower the test plate, with its plane horizontal, on to the surface of the solder in the solder bath (5.1) which is maintained at 300 “C I 5 OC. 3 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 21:44:30 MDTNo reproduction or networking permitted without license from IHS -,-,- After 5 s, remove the test plate from the solder bath, keeping it in a horizontal plane until it has cooled to room temperature. Remove the flux residue with a suitable solvent. Determine the area, in mm2, covered by the melted solder alloy by use of the planimeter (5.3), or measure the height of the solder by use of a micrometer (5.6) and calculate the ratio of spread given in o / o by the formula: xloo Ratio of spread (%) = - D-H D where H is the height of spread solder, in millimetres; D is the diameter, in millimetres, when the solder used is considered as a sphere, D = 1,24 x V V is the volume, in millilitres, of the solder used. 7.3 Replicate tests Using the remaining nine test plates, re-prepare as described in 7.1, repeat the test method described in 7.2, calculating either the area or the ratio of spread as in the original sample. 8 Expression of results The efficacy of the flux sample under test is expressed as the arithmetic mean and the standard deviation of the ten areas or ratios of spread, in mm2, measured in the tests carried out as described in clause 7. The efficacy of the flux sample under test may also be expressed in comparison with results obtained by using the test described in clause 7 on a standard flux, prepared as described in annex A. 9 Precision Interlaboratory tests were carried out on two colophony fluxes without addition of halide and with 0,6 % added halide. Nine laboratories took pari in the tests with the results given in tables 1 to 3. Table 1 - Precision for halide- and non-halide-type fluxes Parameter Arithmetic mean in mm2 Standard deviations - within laboratory - between laboratories Repeatability Reproducibility Flux type 1.1.2 0,6 YO halide 283, i 34,4 62,a 96,4 175,7 Flux type 1.1.3 non halide 155,7 14,3 20,4 40,O 57,2 I 1) The evaluation is based on single values. 4 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 21:44:30 MDTNo reproduction or networking permitted without license from IHS -,-,- o IS0 'b 18,42 r 20,84 IR 51,58 Parameter Arithmetic mean m Standard deviations within sw laboratory - STD-IS0 9955-3O-ENGL 1798 4853903 0755907 397 Area of Ratio of Area of spread spread spread 42,17 55,12 146,02 545 4,lO 4,22 IS0 9455-10:1998() Area of Ratio of spread spread 124,17 80,40 6,36 1,39 23.89 4,37 17,82 3,89 66.89 12.23 Table 2 - Precision for ratio of spread values on brass plates Area of spread 214,23 18,12 25,31 50,74 70.87 Arithmetic mean in mm2 Standard deviations - within laboratory Area of spread 224,21 11.22 21,lO 31,41 59,08 - between laboratories Repeatability Reproducibi
