INTERNATIONAL Iso STANDARD 8502-2 First edition 1982-08-15 Preparation of steel substrates before application of paints and related products — Tests for the assessment of surface cleanliness — Part 2: Laboratory determination of chloride on cleaned surfaces Préparation des subjectiles d’acier avant application de peintures et de Produits assimilés — Essais pour apprécier Ja propreté d'une surface — Partie 2: Recherche des chlorures sur les surfaces nettoyées COPIA LEGAL AUTORIZADA por convenlo con [RAM testituta Argentino de Normalizacién CEWWTRO DE NOCUMENTACION Reforence number 180 8502-2:1992(6)180 8502-2:1992(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards 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 Fepresented on that committee. International organizations, govern- mental and non-governmental, in liaison with ISO. also take part in the work. 180 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 Inter- national Standard requires approval by at least 75% of the member bodies casting a vote. International Standard {SO 8502-2 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Sub-Committee SC 12, Preparation of steel substrates before application of paints and related products. 1SO 8502 consists of the following parts, under the general title Prep- aration of steel substrates before application of paints and related prod- ucts — Tests for the assessment of surface cleanliness: — Part 1: Field test for soluble iron corrosion products [Technical Report] — Part 2: Laboratory determination of chloride on cleaned surfaces — Part 8: Assessment of dust on steel surfaces prepared for painting (pressure-sensitive tape method) ~ Part 4: Guidance on the estimation of the probability of condensation prior to paint application — Part 5: Measurement of chloride on stee! surfaces prepared for painting — fon detector tube method — Part 6: Sampling of soluble impurities on surfaces to be painted — Bresle method ~ Part 7: Analysis of soluble impurities on surfaces to be painted — Analysis methods for field use for chloride © 180. 1992 All rights reserved. No part of this publication may be repraduced or wilized in any form or by any means, slactronlc oF mechanical, including photocopying and mlerotim, without permission in writing from the publisher International Organization tor Stancardization Case Postale 88 CH-1211 Genave 20 # Switzerland Printed tn SwitzerlanaISO 8502-2:1992(E) — Part 8: Analysis of soluble impurities on surfaces to be painted — Analysis methods for fields use for sulfate — Part 9: Analysis of soluble impurities on surfaces to be painted — Analysis methods for field use for ferrous salts — Part 10: Analysis of soluble impurities on surfaces to be painted — Analysis methods for field use for oil and grease — Part 11: Analysis of soluble impurities on surfaces to be painted — Analysis methods for field use for moisture Users should note that the titles to future parts 5 to 11 are working titles, only and that, while itis at present planned to publish all the parts listed above, one or more may nevertheless be deleted from the work pro- gramme before publication, which may, in turn, lead to renumbering of the remaining parts180 8502-2:1992(E) Introduction The performance of protective coatings of paint and related products, applied to steel is significantly affected by the state of the steel surface Immediately prior to painting. The principal factors that are known to Influence this performance are: a) the presence of rust and mill scale; b) the presence of surface contaminants, including salts, dust, oils and greases; ©) the surface profile, International Standards 180 8501, ISO 8502 and ISO 8503: heve been prepared to provide methods of assessing these factors, while ISO 8504 provides guidance on the preparation methods that are available for cleaning steel substrates, indicating the capabilities of each in attaining specified levels of cleanliness. ‘These International Standards do not contain recommendations for the protective coating systems to be applied to the steel surface, Neither do they contain recommendations for the surface quality requirements for specific situations even though surface quality can have a direct influ- ence on the choice of protective coating to-be applied and on its per- formance. Such recommendations are found in other documents such as national standards and codes of practice. it will be necessary for the users of these International Standards to ensure that the qualities specified are: — compatible and appropriate both for the environmental conditions to which the steel will be exposed and for the protective coating system to be used; — within the capability of the cleaning procedure specified. The four International Standards referred to above deal with the follow- ing aspects of preparation of steel substrates: 180 8501 — Visual assessment of surface cleanliness; 180 8502 — Tests for the assessment of surface cleanliness; 180 8503 — Surface roughness characteristics of blast-cleaned steel substrates; 180 8504 — Surface preparation methods. Each of these International Standards is in turn divided into separate parts,ISO 8502-2:1992(E) This part of 130 8502 describes a method for the assessment of chloride-containing salts that are readily soluble in water and are pres- ent on a steel surface. Rusted steel substrates, particularly of rust grades C or D (see ISO 8501-1), evan when blast-cleaned to preparation grade Sa 3 (see 180 8501-1 and ISO 8501-2), may still be contaminated by soluble salts and corrosion products. These compounds are almost colourless and are localized at the lowest point of the rust pits. If they are not removed prior to painting, chemical reactions can result In large accumulations of rust that desiroy the adhesion between the substrate and the applied protective coating. Even if the salt is readily soluble in water, it is often impossible to re- move it completely from the surface by a simple washing such as that described in this procedure. The method does not therefore determine the total amount of chloride on the surface but gives an indication of the cleanliness level of the surface. Careful scraping of the surface with a metal spatula or knife during the washing, and prolonging the washing time, should remove a larger proportion:of the salt.INTERNATIONAL STANDARD ISO 9502-2:1992(E) Preparation of steel substrates before applica in of paints and related products — Tests for the assessment of surface cleanliness — Part 2: Laboratory determination of chloride on cleaned surfaces WARNING — The procedure described in this part of ISO 8502 Is Intended to be carriod out by qualified ‘chem! use in this. or by other suitably trained and/or supervised personnel. The substances and procedures ithod may be injurious to health if adequate precautions are not taken. Attention Is drawn in the text (see 4.4) to certain specific hazards. This part of SO 8502 refers only to Its technical suitability and does not absolve the user from statutory obligations relating to health and safety. 1 Scope This part of 180 8502 describes a method for as- sessment of chioride-containing salts that are read- lly soluble in water and are present on a steel surface. The method Is also applicable to previously coated surfaces. It is normally to be used in a lab- ‘oratory using washings sampled from surfaces on site. The method is applicable to the assessment of salts that have been introduced by the cleaning pro- cedure, or that have deposited on the surface before or after the cleaning. NOTE 1 Although the procedure for chloride determi- nation ia generally accurate, the overall precision of the method is limited by uncertainties in the sampling pro- ‘cedure, In addition, traces of iron chloride at the bottom of pits are difficult to extract into the sample. The test method cannot be used on surfaces treated with chromate or nitrite, which are commonly used as inhibitors in the water when wet blast-cleaning This is because a chromate concentration of 10 mg/l or greater or a nitrite concentration of 20 mg/l or greater in the wash water interferes with the determination of the chloride. An ironi{ll) ion concentration of 10 mg/l also inter- eres with the determination, but the iron({t!) lons are concentrated in the rust deposits, which are re~ moved from the test solution by filtration. 2 Normative references The following standards. contain provisions which, through reference in this text, constitute provisions of this part of ISO 8502. 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 8502 are encouraged to investi- gate the possibility of applying the most recent edi- tions of the standards indicated below. Members of IEC and 180 maintain registers of currently valid International Standards. 180 3698:1987, Water for analytical laboratory use — Specification and test methods. 180 8501-1:1988, Preparation of stee! substrates be- fore application of paints and related products — Visual assessment of surface cleanliness — Part 1: Rust grades and preparation grades of uncoated steel substrates and of steel substrates after overall removal of previous coatings.ISO 8502-2:1992(E) 180 8501-2:—, Preparation of steel substrates before application of paints and related products — Visual assessment of surface cleanliness — Part 2: Prep- aration grades of previously coated stee! substrates after localized removal of previous coatings. 3. Principle A defined area of the steel surface is washed with a known volume of water and the chloride in the wash water is titrated with mercury(l) nitrate using a. diphenylcarbazone/bromophenol blue _mixed- indicator titration method developed by Clarke. In the titration, mercury ions react with free chloride ions to form HgCl, which dissociates only slightly. When the chloride ions are consumed, the excess mercury ions give an. intense violet colour with diphenylcarbazone, thus Indicating the end-point of the titration, 4 Reagents During the analysis, use only reagents of recognized analytical grade. and water of at least grade 3 purity in accordance with [SO 3696. 4.4. Nitric acid, c(HNO,) about 0,05 mol}! Add 3,5ml- of. concentrated nitric. acid (p= 1,40 gjml) to. some water, and make up: to 1.000.ml with water. 4.2 Sodium hydroxide soliton, (NaOH) ‘about 0,025 molfl Dissolve 1,0 g of sodium hydroxide in water: transfer to a 1.000 mi volumetric flask and make uo to the mark with water. 4.3 Potassium chloride, standard solution, p(Cl) = 100 mg/t. Dissolve 0,210.39 of potassium chloride in water, transfer to a 1000 mi volumetric flask and make up to the mark with water, 1 ml of this solution contains 0,1 mg of Cl. 44 Mercury(il) nitrate, standard volumetric sol- ution, efHg(NO,),] = 0,012 5 mol/l. WARNING — Mercury(I!) nitrate is toxic. Avoid con- tact with eyes and skin. 1) To be published. 4.41 Preparation Dissolve 4.171 g of mercury(ll) nitrate hemihydrate, [Hg(NO,)2.0,5H,0] in water, transfer to a 1000 mi volumetric flask and make up to the mark with wa- ter. 4.4.2, Standardization Introduce by means.of a pipette (5.11) into a beaker (5.5) a 20 ml aliquot of the potassium chloride stan- dard solution (4.3). Add 5 drops of the diphenyl- carbazone/bromophenol blue mixed-indicator sol- ution (4.8) and stir. Ia blue-violet or red colour de- velops, add nitric acid (4.1) dropwise until the colour changes to yellow and then add 1 ml excess of nitric acid. If a yellow or orange colour forms immediately on the addition of the indicator, obtain the blue-violet colour by adding sodium hydroxide solution (4:2) dropwise. Then proceed with the acidification Titrate the yellow acidified solution with the mercury(t!) nitrate solution (4.4) until, a. blue-violet colour persists throughout the solution: Retain the titrated solution for comparison with the blank titrated solution obtained: in 6.1. Calculate: the: con- centration:of the. mercury(I) nitrate. solution. Note that 1 mol of mercury) fons Is equivalent fo 2 mol of chloride ions, 45 Diphenyearbazone/oromophenol blue, mixed- indicator solution. Dissolve 0,5 g of crystalline diphenylcarbazone and 0,05 g of crystalline bromophenol blue in 75'ml of ethanol, 95 °% (V/V), and make up to 100 mi-with ethanol. Store in a brown bottle. 5 Apparatus and materials 5.4 Ruler and essentially chloride-free chalk, or other suitable means for marking the test area. 5.2 Absorbent cotton pads (cotton wool), of mass. 1gto15¢ 5.3 Metal spatula or knife, 5.4 Gloves, of plastics material 8.5. Beakers, of capacity 250 ml 5.6 Small glass rod. 57 Funnel, 2) CLARKE, F.E, : Determination of chloride in water, Analytical Chemistry, 22 (1950), 4, pp. 653-855.5.8 Filter paper, approximately 120 mm diameter. 5.9 Measuring cylinder, of capacity 50 ml. 5.10 Volumetric flasks, of capacity 50 ml, 100 ml and 1.000 mi. 5.11 Volumetric pipettes, of capacity 1 ml and 20 mi. 5.12. Device for titration, preferably a digital titrator. 6 Procedure 6.1. Blank titration Carry out a blank titration each time on water, re- taining the titrated solution for comparison of end- points. Follow the procedure described in’ 4.4.2 but using 20 ml of water instead of the potassium chlor- ide solution. 6.2. Washing of the surface Carry out the test at least.in duplicate. During the swabbing procedure, ensure absence of accidental, contamination of the wash water by using, for ex- ample, clean plastic gloves (5.4). Mark out a test area measuring approximately 25 000 mm® (for example 250 mm x 100 mm) using the ruler and chalk or other suitable means (5.1). Mark two beakers (5.5) A and B. Pour 45 ml of water into beaker A, using the measuring cylinder (5.9). Soak an absorbent cotton pad (5.2) In the water and thoroughly swab the test area with the pad. Do not allow water to drip ftom the pador run off the test afea, Remove the water from the surface with. the absorbent cotton. pad and squeeze the washings into beaker B. In the case of bare steel, scrape the surface with the metal spatula or knife (6.3) untit bright metal Is ex- posed over at least 50 % of the test area. Repeat the swabbing procedure with several portions of water and, if the pad is worn.out, use a fresh one, continuing. in this way until all the water has been used up. Keep the used absorbent cotton pads. The swabbing procedure should take at least 5 min. ¢ Filter the washings, using the filter paper (5.8) and the funnel (5.7), and collect the filtrate in. the volumetric flask of capacity 50 ml (5,10). Wash the Used absorbent cotton pads and the filter papers with. small portions of water (total 5 mi), using beaker B and the small glass rod (5.6). Squeeze the pads and collect the washings in the flask. Make up to the mark with water. 180 9502-2:1992(E) 63 Wash-water titration Carefully shake the 50 ml volumetric flask. Using a pipette (5.11), transfer 20 mi of the wash water into aclean beaker (5.5). Determine the chloride content by following the procedure given in 4.4.2 but using the wash water. 7 Expression of results Calculate the assessed amount of chloride per unit surface area, p4(Cl), expressed in milligrams per square metre, using the equation (Hy = Vole 1,773 x 10° eC) = 7 where V, Is the volume, expressed In millilitres, of the mercury) nitrate solution used for ‘the titration of the wash water (see 6.3); Yo is the volume, expressed In millilitres, of the mercury(li) nitrate solution used for the blank titration (see 6.1); © is the actual concentration, expressed in moles of Hg(NO2), per litre, of the mercury(ll) nitrate solution, as deter- thined in 4.42; A isthe surface area washed, expressed In ‘square millimetres Report each result to the nearest 10. mg/m”. NOTE2 The performance of a paint system is affected ty the amount of soluble chloride remaining on the su face, The acceptable level of this contamination is related 19 the service conditions’ Experience in the use of tt ‘nethod is limited and moro will be needed before limits, ‘can be specified in connection with its use. 8 Test report ‘The test report shall contain at least the following information: a) all details. necessary: to identify the surface tested, including detalls of shape and attitude (e.g. horizontal, vertical, at an angle); b) a reference to this part of ISO 8502 (ISO 8502-2): ¢) the results of the test, as indicated in clause 7; 4) any deviation from the test method specified; e) the date(s) of the test.10 8502-2:1992(E) 1 } | UDC 667.648.1:669.14:620.179,11 Descriptors: paints, varnishes, substrates, stesl products, tests, laboratory tests, determination, surface condition, cleantinass checks, chlorides. Price based on 9 pages