1、BSI Standards PublicationBS EN 4503:2013Aerospace series Non-metallic materials Textiles Test method Determinationof water soluble chloride andsulfate of aqueous extractsBS EN 4503:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 4503:2013.The UK participati
2、on in its preparation was entrusted to TechnicalCommittee ACE/65, Non-metallic materials for aerospace purposes.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Use
3、rs are responsible for its correctapplication. The British Standards Institution 2013. Published by BSI StandardsLimited 2013ISBN 978 0 580 81723 6ICS 49.025.60Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of t
4、heStandards Policy and Strategy Committee on 31 July 2013.Amendments issued since publicationDate Text affectedBS EN 4503:2013EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 4503 July 2013 ICS 49.025.60 English Version Aerospace series - Non-metallic materials - Textiles - Test method - Determi
5、nation of water soluble chloride and sulfate of aqueous extracts Srie arospatiale - Matriaux non-mtalliques - Textiles - Mthode dessai - Dtermination des chlorures et des sulfates des rsidus aqueux Luft- und Raumfahrt - Nichtmetallische Werkstoffe - Textilien - Prfverfahren - Bestimmung von wasserls
6、lichem Chlorid und Sulfat in wsserigen Lsungen This European Standard was approved by CEN on 8 May 2013. 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 alteration
7、. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by t
8、ranslation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Fi
9、nland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZA
10、TION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 4503:2013: EBS EN 4503:2013EN 4503:2013 (E) 2 Contents Pag
11、e Foreword . 3 Introduction. 4 1 Scope 5 2 Normative references . 5 3 Terms and definitions 5 4 Health, safety and environment . 6 5 Principle/Technique . 6 6 Resources. 6 7 Test samples/test pieces . 7 8 Test procedure . 8 9 Expression of results . 9 10 Measurement uncertainties . 10 11 Designation
12、 10 12 Test report 10 BS EN 4503:2013EN 4503:2013 (E) 3 Foreword This document (EN 4503:2013) has been prepared by the Aerospace and Defence Industries Association of Europe - Standardization (ASD-STAN). After enquiries and votes carried out in accordance with the rules of this Association, this Sta
13、ndard has received the approval of the National Associations and the Official Services of the member countries of ASD, prior to its presentation to CEN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the lates
14、t by January 2014, and conflicting national standards shall be withdrawn at the latest by January 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all su
15、ch patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Mace
16、donia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 4503:2013EN 4503:2013 (E) 4 Introduction This standard is part
17、of the series of EN non-metallic materials standards for aerospace applications. The general organisation of this series is described in EN 4385. This standard is a level 3 document as defined in EN 4385. BS EN 4503:2013EN 4503:2013 (E) 5 1 Scope This European Standard specifies the determination of
18、 water soluble chloride and sulphate of aqueous extracts of textile materials. This method has been written in response to an aerospace requirement for a method of extraction using hot water, this method should be used in conjunction with EN 4426. 2 Normative references The following documents, in w
19、hole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 4385, Aerospace series Non-metall
20、ic materials General organisation of standardization Links between types of standards EN 4426, Aerospace series Non-metallic materials Textiles Test method Determination of conductivity and pH of aqueous extracts 1)EN 20139, Textiles Standard atmospheres for conditioning and testing (ISO 139) EN ISO
21、 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) ISO 383, Laboratory glassware Interchangeable conical ground joints ISO 4793, Laboratory sintered (fritted) filters Porosity grading, classification and designation 3 Terms and definitions For the purposes of this d
22、ocument, the following terms and definitions apply. 3.1 chloride free water soluble Clion which could combine with free H+ions to produce acidic conditions which would be detrimental to the ageing of fabrics 3.2 sulfates free water soluble SO4C ion which could combine with free H+ ions to produce ac
23、idic conditions which would be detrimental to the ageing of fabrics 1) Published as ASD-STAN Prestandard at the date of publication of this standard BS EN 4503:2013EN 4503:2013 (E) 6 4 Health, safety and environment This standard does not necessarily include all health and safety requirements associ
24、ated with its use. Persons using this standard shall be familiar with normal laboratory/test house practices. It is the responsibility of the user to establish satisfactory health and safety practices and to ensure conformity with any European, National or local laws/regulations. 5 Principle/Techniq
25、ue An aqueous extract is prepared using distilled water. The soluble chloride and sulphate are then measured by gravimetric method. A volumetric method may also be used to determine the amount of soluble chloride. 6 Resources 6.1 Apparatus/facilities 6.1.1 Round bottomed flasks of chemically resista
26、nt glass with a volume of 250 ml and a ground glass neck of size 24/29 in accordance with ISO 383 6.1.2 A glass stopper incorporating a stopcock with P.T.F.E. core liner to prevent sticking of the glass core in the neck of the stopcock NOTE Grease shall not be used for this purpose. 6.1.3 Water-cool
27、ed condensers 6.1.4 Laboratory balance, accurate to 0,000 2 g 6.1.5 Sinter glass crucibles, porosity 4 in accordance with ISO 4793 6.1.6 Titration vessel and reference half-cell, with suitable pH meter as used with glass electrodes, set to read in mV NOTE The half-cell is filled with silver oxalate
28、suspension. 6.1.7 Sintered porcelain or silica gooch filter crucibles, porosity 4 in accordance with ISO 4793 6.1.8 Filter paper with the following nominal characteristics: mass of 100 g/m2 retention 2,5 m initial filtration speed slow thickness 0,2 mm ash content 0,007 % NOTE Whatman 42 has been fo
29、und suitable. BS EN 4503:2013EN 4503:2013 (E) 7 6.2 Materials/reagents The following reagents are required and shall be of recognized analytical quality. 6.2.1 Potassium chloride solution, of concentration 0,001 mol/1, which has a conductivity of 12,780 mS/m at 20 C 6.2.2 Distilled or deionized wate
30、r, in accordance with EN ISO 3696. It should have a maximum conductivity of 1 mS/m. For pH determinations remove carbon dioxide from the water by boiling for 5 min, then cool in the absence of air before use. 6.2.3 Silver oxalate suspension, made by dissolving 14 g of sodium oxalate and 10 g of pota
31、ssium nitrate in 1 litre of water (6.2.2) adding with constant stirring, 100 ml of silver nitrate (7.2.7). The stock suspension shall be kept in a dark glass bottle. 6.2.4 Nitric acid solution, concentrated 6.2.5 Nitric acid solution, approximately 0,5 % v/v 6.2.6 Nitric acid solution, approximately
32、 10 % v/v 6.2.7 Silver nitrate solution, 0,1 mol/l 6.2.8 Silver nitrate solution, 0,01 mol/l 6.2.9 Sodium chloride solution, approximately 100 g/l 6.2.10 Hydrochloric acid solution, concentrated 6.2.11 Barium chloride solution, 20 g/l 6.3 Qualification of personnel No specific technical requirements
33、. 7 Test samples/test pieces Samples shall be taken representative of the bulk and of sufficient size to provide all the test specimens required. All samples shall be kept identifiable to the bulk textiles which they represent. Cut the sample under test into pieces of such size that all parts readil
34、y wet out. Care shall be taken to avoid contamination of samples and handling shall be kept to an absolute minimum. NOTE Nominal 10 mm squares have been found suitable. The samples are conditioned and tested in a standard atmosphere of (65 2) % r.h. and (20 2) C in accordance with EN 20139 Standard
35、Temperate Atmosphere For Testing. BS EN 4503:2013EN 4503:2013 (E) 8 8 Test procedure 8.1 Preparation Cut the sample into nominal 10 mm squares and weigh (5 0,05) g of conditioned sample into flask (6.1.1). To the flask containing the sample under test add (100 0,1) ml of distilled water (6.2.2). NOT
36、E For sample weight of less than 5 g, the liquor ratio should be maintained at 1: 20, i.e. 1 g of sample to 20 ml of water. Connect the flask containing the sample and water to the water cooled condenser (6.1.3). Quickly bring contents to the boil and continue to boil liquor gently for 60 minutes. A
37、fter this period disconnect and remove flask from the condenser whilst liquor is still boiling close immediately with the glass stopcock (6.1.2). Do not filter or make up volume but cool rapidly to (20 2) C to ensure partial vacuum is created to ensure the extract is not contaminated. 8.2 Determinat
38、ion of water soluble chloride 8.2.1 Gravimetric method. Prepare an extract as described in 8.1 If the textile contains chlorinated compounds, e.g. PCPL, carry out a preliminary extraction with a suitable solvent before preparing the extract as described in 8.1. Take a suitable measured portion, add
39、5 ml of concentrated nitric acid (6.2.4) per 100 ml of extract boil for 5 min and leave overnight. Filter through a filter paper pulp pad, wash with distilled water, and add a slight excess of silver nitrate solution (6.2.7) to the combined filtrate and washings. Heat the solution, protected from di
40、rect light, in a water bath until the precipitate is coagulated and the supernatant liquor is clear. Verify completeness of precipitation by adding a drop of silver nitrate solution (6.2.7) to the supernatant liquor. Allow to cool in the dark, and then filter through a tarred crucible (6.1.5). Wash
41、the crucible with dilute nitric acid (6.2.5) until the washings give no opalescence when tested with sodium chloride solution (6.2.9). Then dry the crucible initially at about 100 C and finally to constant mass 2)at 130 C to 150 C. Carry out a blank determination and subtract the mass thus obtained
42、from the mass obtained in the test. Calculate the water-soluble chlorides as described in .9.2.1.1. 8.2.2 Volumetric method. Before each test, verify that all parts of the apparatus are clean. Clean the silver wire electrodes with very fine abrasive or use a suitable chemical method. Discard and rep
43、lace the silver oxalate suspension (6.2.3) at the first sign of darkening; to delay darkening, shield the half-cell from light when not in use. Shake the suspension bottle thoroughly before replenishing the half-cell. Take particular care that electrolytes do not come into contact with the junctions
44、 between the silver wire electrodes and their leads to the pH meter. Flush the electrolyte junction after each determination by easing the stopper at the bottom of the half-cell to allow fresh oxalate suspension (6.2.3) to flow into the junction. Prepare an extract as described in 8.1. Take a suitab
45、le measured portion (a suitable test portion should contain a minimum of 0,2 mg of chloride ion), add 1 ml of nitric acid (6.2.6) per 100 ml of extract, boil for 5 min, cool rapidly to room temperature and transfer to the titration vessel. Start the stirrer, connect the electrodes to the pH meter, s
46、et to read in mV, and titrate with silver nitrate solution (6.2.8) until a reading of 0 mV is first indicated. Carry out a blank determination and calculate the water soluble chlorides as described in 9.2.1.2. 8.3 Determination of water-soluble sulfates by gravimetric analysis Prepare an extract as
47、described in 8.1. Take a measured portion, filter through a suitable filter paper (6.1.8) and wash with distilled water. Add concentrated hydrochloric acid (6.2.10) drop by drop until the solution is just acid to litmus, then add 1 ml of acid per 100 ml solution. Boil for 5 min and leave to cool ove
48、rnight. Filter off any precipitate on a filter-paper pulp pad, wash with distilled water and heat the combined filtrate and washings to boiling. While still boiling add, drop by drop, 10 ml of hot barium chloride solution (6.2.11). 2) That is until the residue suffers no more than 0,0005 g loss of m
49、ass on drying for a further 30 min. BS EN 4503:2013EN 4503:2013 (E) 9 Continue boiling for 30 min, then leave to cool overnight. Transfer the precipitate quantitatively to a crucible (6.1.5), and wash with cold water (6.2.2) until the washings are free from chloride. Heat the crucible and its contents, gently at first, and finally to constant mass* at 800 C to 900 C. Carry out a blank determination and calculate the water-soluble sulphates as described in 9.2.2. 9 Expression of results 9.1 Individual results S
