1、BRITISH STANDARD BS EN ISO 3549:2002 Incorporating Amendment No. 1 to BS 3982:1996 (renumbers the BS as BS EN ISO 3549:2002) Zinc dust pigments for paints Specifications and test methods The European Standard EN ISO 3549:2002 has the status of a British Standard ICS 87.060.10 BS EN ISO 3549:2002 Thi
2、s British Standard, having been prepared under the direction of the Sector Board for Materials and Chemicals, was published under the authority of the Standards Board and comes into effect on 15 May 1996 BSI 12 February 2003 The following BSI references relate to the work on this standard: Committee
3、 reference STI/1 Draft for comment 90/55444 DC ISBN 0 580 25577 8 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee STI/1, Pigments, upon which the following bodies were represented: British Cement Association British Coati
4、ngs Federation Ltd. British Colour Makers Association British Precast Concrete Federation Ltd. British Ready Mixed Concrete Association Cement and Concrete Pigment Suppliers Association China Clay Association Oil and Colour Chemists Association Titanium Pigment Manufacturers Technical Committee Zinc
5、 Development Association Amendments issued since publication Amd. No. Date Comments 14167 12 February 2003 Implementation of the European StandardBS EN ISO 3549:2002 BSI 12 February 2003 i Contents Page Committees responsible Inside front cover National foreword ii 1S c o p e 1 2 Normative reference
6、s 1 3 Definition 1 4 Required characteristics and tolerances 1 5 Sampling 2 6 Determination of residue on sieve 2 7 Determination of total zinc content 4 8 Determination of metallic zinc content 6 9 Determination of lead, cadmium and iron content 7 10 Determination of arsenic content 10 11 Determina
7、tion of chloride content 14 12 Determination of matter insoluble in acid 15 13 Test report 15 Figure 1 Air-jet sieve apparatus 3 Figure 2 Example of hydride generation apparatus 13 Table 1 Composition of zinc dust pigment 1 Table 2 Residue on sieve 1BS EN ISO 3549:2002 ii BSI 12 February 2003 Nation
8、al foreword This British Standard is the official English language version of EN ISO 3549:2002. It is identical with ISO 3549:1995. The UK participation in its preparation was entrusted to Technical Committee STI/1, Pigments, which has the responsibility to: A list of organizations represented on th
9、is committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled International Standards Correspondence Index, or by using
10、the Search facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from l
11、egal obligations. 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 promulgate them in the UK.
12、 Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN ISO title page, the EN ISO foreword page, pages 1 to 16, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.EUROP
13、EAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 3549 September 2002 ICS 87.060.10 English version Zinc dust pigments for paints Specifications and test methods (ISO 3549:1995) Pigments base de poussire de zinc pour peintures Spcifications et mthodes dessai (ISO 3549:1995) Zinkstaub-Pigmente fr B
14、eschichtungsstoffe Anforderungen und Prfverfahren (ISO 3549:1995) This European Standard was approved by CEN on 21 July 2002. 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 w
15、ithout any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language
16、made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland
17、, Ireland, Italy, Luxembourg, Malta, 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 2002 CEN All rights of
18、exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 3549:2002 EEN ISO 3549:2002 BSI 12 February 2003 Foreword The text of ISO 3549:1995 has been prepared by Technical Committee ISO/TC 35, Paints and varnishes, of the International Organization for S
19、tandardization (ISO) and has been taken over as EN ISO 3549:2002 by Technical Committee CEN/TC 298, Pigments and extenders, the Secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement,
20、at the latest by March 2003, and conflicting national standards shall be withdrawn at the latest by March 2003. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Re
21、public, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom.EN ISO 3549:2002 BSI 12 February 2003 1 1 Scope This International Standard specifies the requirements and corresponding tes
22、t methods for zinc dust pigments suitable for use in protective coatings. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All
23、standards are subject to revision, and parties to agreements based on this International Standard are encouraged 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.
24、 ISO 565:1990, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings ISO 594-1:1986, Conical fittings with a 6 % (Luer) taper for syringes, needles and certain other medical equipment Part 1: General requirements ISO 842:1984, Raw materials for paints
25、 and varnishes Sampling ISO 3696:1987, Water for analytical laboratory use Specification and test methods 3 Definition For the purposes of this International Standard, the following definition applies. 3.1 zinc dust pigment a fine grey powder of essentially spheroidal particles, mainly consisting of
26、 metallic zinc NOTE 1 Zinc dust pigments for paints may vary in their metallic zinc content, chemical purity, particle shape, particle size distribution, mean and maximum diameter, etc. These variations are all likely to have an influence on the zinc dust behaviour in paints with regard to parameter
27、s such as dispersibility, fineness of grind, reactivity, electrical conductivity and packing properties. 4 Required characteristics and tolerances 4.1 For zinc dust pigments complying with this International Standard, the essential requirements are specified in Table 1 and Table 2. Table 1 Compositi
28、on of zinc dust pigmentTable 2 Residue on sieve Characteristic Unit Requirement Test method Total zinc content % (m/m) min. 98 see Clause 7 Metallic zinc content % (m/m) min. 94 see Clause 8 Lead (Pb) content % (m/m) max. 0,2 see Clause 9 Cadmium (Cd) content % (m/m) max. 0,1 see Clause 9 Iron (Fe)
29、content % (m/m) max. 0,05 see Clause 9 Arsenic (As) content % (m/m) max. 0,000 5 see Clause 10 Chloride (Cl) content % (m/m) max. 0,005 see Clause 11 Matter insoluble in acid % (m/m) max. 0,05 see Clause 12 NOTE If the zinc oxide content is required, this can be calculated by multiplying the differe
30、nce between the total zinc content and the metallic zinc content by 1,244 7. Nominal size of sieve aperture m Residue on sieve % (m/m) Test method 125 max. 0,01 90 max. 0,1 See Clause 6 45 max. 5EN ISO 3549:2002 2 BSI 12 February 2003 4.2 Requirements for other physical properties (surface area, par
31、ticle size distribution, etc.) and the choice of reference pigment to which these properties refer shall be the subject of agreement between the interested parties. 4.3 The reference pigment shall also comply with the requirements given in Table 1 and Table 2. 5 Sampling Take a representative sample
32、 of the product to be tested, as described in ISO 842. WARNING The sample shall on no account be dried before testing, and any portion of the sample not used shall not be returned to the sample container after having been manipulated. 6 Determination of residue on sieve 6.1 Principle A suitable test
33、 portion of the sample is passed through an air-jet sieve apparatus having sieves with nominal mesh apertures of 45 m, 90 m and 125 m. The residue on each of these sieves is determined. 6.2 Apparatus 6.2.1 Sieves, circular, with a sieving area of diameter 200 mm and with nominal mesh apertures of 45
34、 m, 90 m and 125 m, complying with ISO 565. A transparent lid shall be provided to cover the sieve during use. 6.2.2 Air-jet sieve apparatus (see Figure 1), consisting of a cylindrical casing which contains a sieve (see 6.2.1). The base of the casing has an outlet (to which an extractor fan is conne
35、cted) and an air inlet to permit the injection of air. The air inlet is connected to a jet rotating at 20 r/min to 25 r/min and consists of a slot-shaped nozzle located beneath and very close to the sieve (see Figure 1). When the jet rotates, it blows air continuously through the sieve, preventing t
36、he powder particles from settling. The air is extracted through the outlet, drawing the finer particles through the sieve. The flow of air is controlled by adjusting a slot at the outlet. The vacuum obtained shall be 1 250 Pa or better. 6.2.3 Timer (for example a stopwatch), recording to the nearest
37、 1 s or better. It may be equipped with a switch for stopping the motor of the sieve apparatus (6.2.2). 6.2.4 Analytical balance, capable of weighing at least 50 g to the nearest 1 mg. 6.2.5 Mallet, of light construction, with a plastic head, suitable for tapping the apparatus to dislodge powder adh
38、ering to the lid and sieve. 6.2.6 Clean brush 6.2.7 Stainless-steel boat 6.3 Checking and cleaning the sieve Check that the sieve is clean and undamaged and is not blocked by material used in a previous determination. A magnifying glass of sufficient magnification is recommended to aid this inspecti
39、on. If cleaning of the sieve is necessary, an ultrasonic system is recommended for this purpose. It is also possible to clean the sieve by turning it upside down on a clean sheet of paper and tapping vigorously to eliminate any residual particles.EN ISO 3549:2002 BSI 12 February 2003 3 6.4 Procedure
40、 Carry out the determination in duplicate. 6.4.1 Weigh, to the nearest 0,01 g, a test portion of approximately 50 g (m 0 ). 6.4.2 Secure the 45 m sieve (6.2.1) in position in the sieve apparatus (6.2.2) and transfer the test portion to the sieve. 6.4.3 Cover the sieve with the transparent lid, switc
41、h on the extractor fan and sieve apparatus (6.2.2) and tap the lid and the sieve lightly from time to time with the mallet (6.2.5) to distribute the material and dislodge adhering particles. 6.4.4 After 120 s, switch off the apparatus and remove the transparent lid and sieve. Recover the sieve resid
42、ue by turning the sieve upside down on a clean sheet of paper and tapping vigorously to ensure that all particles are recovered. 6.4.5 Weigh the stainless-steel boat (6.2.7) to the nearest 1 mg (m 1 ). Transfer the sieve residue to it and reweigh to the nearest 1 mg (m 2 ). 6.4.6 Repeat the operatio
43、ns described in 6.4.1, 6.4.2, 6.4.3, 6.4.4 and 6.4.5 with the 90 m sieve and then with the 125 m sieve on fresh 50 g portions of the sample. Figure 1 Air-jet sieve apparatusEN ISO 3549:2002 4 BSI 12 February 2003 6.5 Expression of results Calculate the residue on each sieve, R, expressed as a percen
44、tage by mass, using the equation If the two results (duplicates) for each sieve differ by more than one tenth of the maximum limit for that sieve in Table 2, repeat the procedure. Calculate the mean of two valid results (replicates) and report the result to three decimal places for the 125 m sieve,
45、two decimal places for the 90 m sieve and one decimal place for the 45 m sieve. 7 Determination of total zinc content 7.1 Principle The zinc is titrated against EDTA solution. 7.2 Reagents During the analysis, use only reagents of recognized analytical grade and only water of at least grade 3 purity
46、 as defined in ISO 3696. 7.2.1 Hydrochloric acid, concentrated, approximately 38 % (m/m), 1,19 g/ml. 7.2.2 Hydrochloric acid, diluted 1 + 4. Dilute 200 ml of concentrated hydrochloric acid (7.2.1) to 1 litre with water. 7.2.3 Sulfuric acid, diluted 1 + 1. Slowly add, whilst cooling, 1 part by volume
47、 of concentrated sulfuric acid approximately 96 % (m/m), 1,84 g/ml to 1 part by volume of water. 7.2.4 Nitric acid, concentrated, approximately 68 % (m/m), 1,42 g/ml. 7.2.5 Ammonia solution, approximately 25 % (m/m), 0,81 g/ml. 7.2.6 Buffer solution Dissolve 200 g of hydroxylammonium chloride (NH 2
48、OH HCl) in approximately 300 ml of water. Dissolve 28 g of sodium hydroxide in approximately 300 ml of water. Combine the two solutions, cool and dilute to 1 litre with water. 7.2.7 (Ethylenedinitrilo)tetraacetic acid (EDTA), disodium salt dihydrate, standard volumetric solution. 7.2.7.1 Preparation
49、 Weigh, to the nearest 1 mg, about 20 g of disodium EDTA dihydrate, dissolve in water and make up to 1 litre. Store in a polyethylene bottle. 7.2.7.2 Standardization Weigh, to the nearest 1 mg, approximately 1,5 g of 99,99 % pure zinc metal (mass m 0 ) into a 250 ml beaker. Dissolve in 20 ml of hydrochloric acid (7.2.1) and add 1 ml or 2 ml of nitric acid (7.2.4). After complete dissoluti
