1、BRITISH STANDARDBS EN50414:2006Test methods for analysis of lead in PVC taken from insulation and sheath of electric and optical fibre cables Method A: Total lead content determination with flame excitation atomic absorption spectrometry Method B: Qualitative analysis of lead by lead sulphide staini
2、ngThe European Standard EN 50414:2006 has the status of a British StandardICS 29.035.20g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 50414:2
3、006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 May 2006 BSI 2006ISBN 0 580 48384 3National forewordThis British Standard is the official English language version of EN 50414:2006.The UK participation in its preparation was entrusted by
4、 Technical Committee GEL/20, Electric cables, to SubcommitteeGEL/20/17, Low voltage cables, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or Eur
5、opean publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include a
6、ll 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 legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries
7、on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.Summary of pagesThis document comprises a front cover, an inside front cover, the EN title page, pages 2 to 11 and a back cover.The BS
8、I copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsEUROPEAN STANDARD EN 50414 NORME EUROPENNE EUROPISCHE NORM April 2006 CENELEC European Committee for Electrotechnical Standardization Comit Europen de No
9、rmalisation Electrotechnique Europisches Komitee fr Elektrotechnische Normung Central Secretariat: rue de Stassart 35, B - 1050 Brussels 2006 CENELEC - All rights of exploitation in any form and by any means reserved worldwide for CENELEC members. Ref. No. EN 50414:2006 E ICS 29.035.20 English versi
10、on Test methods for analysis of lead in PVC taken from insulation and sheath of electric and optical fibre cables - Method A: Total lead content determination with flame excitation atomic absorption spectrometry - Method B: Qualitative analysis of lead by lead sulphide staining Mthodes danalyse du p
11、lomb dans le PVC prlev de lenveloppe isolante et des gaines des cbles lectriques et fibres optiques - Mthode A: Dtermination de la teneur totale en plomb par spectromtrie atomique dabsorption dans la flamme - Mthode B: Analyse qualitative du plomb par production de sulfure de plomb Prfverfahren fr d
12、ie Analyse von Blei in PVC entnommen aus Isolierung und Mantel von Kabeln, isolierten Leitungen und Lichtwellenleiterkabeln - Verfahren A: Bestimmung des Gesamtbleigehalts mit der Flammen-Atomabsorptionsspektrometrie - Verfahren B: Qualitative Analyse des Bleigehalts durch BleisulfidverfrbungThis Eu
13、ropean Standard was approved by CENELEC on 2006-03-01. CENELEC 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. Up-to-date lists and bibliographical referen
14、ces concerning such national standards may be obtained on application to the Central Secretariat or to any CENELEC member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CENELEC mem
15、ber into its own language and notified to the Central Secretariat has the same status as the official versions. CENELEC members are the national electrotechnical committees of Austria, Belgium, Cyprus, the Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland,
16、 Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. EN 50414:2006 - 2 - Foreword This European Standard was prepared by the Technical Committee CENELEC TC 20, Electric cables. The tex
17、t of the draft was submitted to the formal vote and was approved by CENELEC as EN 50414 on 2006-03-01. The following dates were fixed: latest date by which the EN has to be implemented at national level by publication of an identical national standard or by endorsement (dop) 2007-03-01 latest date b
18、y which the national standards conflicting with the EN have to be withdrawn (dow) 2009-03-01 _ - 3 - EN 50414:2006 Contents Introduction.4 1 Scope 4 2 Normative references .4 3 Methods of analysis .5 3.1 General .5 3.2 Method A.5 3.2.1 Principle 5 3.2.2 Reagents.5 3.2.3 Apparatus6 3.2.4 Sampling .6
19、3.2.5 Test procedure 6 3.2.6 Determination7 3.2.7 Tests results9 3.2.8 Test report.10 3.3 Method B.10 3.3.1 Principle 10 3.3.2 Reagents.10 3.3.3 Apparatus10 3.3.4 Procedure10 3.3.5 Determination11 3.3.6 Test report.11 Table 1 - Preparation of reference solutions8 EN 50414:2006 - 4 - Introduction The
20、 determination of small quantities of lead in PVC is possible using a number of analytical techniques. For the purposes of this European Standard two alternative methods are given. Method A uses flame excitation atomic absorption spectrometry, for the total lead determination in the PVC. Method B us
21、es a qualitative method for the analysis of lead in the PVC. The method utilises the lead sulfide staining test and is therefore best suited to light coloured or natural materials. It can be considered to be a spot check for the presence of lead or lead compounds. Other decomposition and determinati
22、on methods are capable of detecting and analysing small amounts of lead in cable grade PVC. Examples of such methods are X-ray fluorescence spectroscopy, graphite furnace atomic absorption spectrometry, inductively coupled plasma spectrometry and polarography. Contracting parties may agree to use su
23、ch other methods, but such methods cannot claim conformity to EN 50414. If used, it is recommended that such methods have at least equivalent sensitivity and detection levels as those in this EN. 1 Scope This European Standard describes two methods for the analysis of lead in PVC-insulating and shea
24、thing materials for electric and for optical fibre cables. The samples of PVC are taken from the finished cable. Method A provides a quantitative method and Method B provides a qualitative method. NOTE 1 Users may refer to either Method A or Method B or to both methods. NOTE 2 Other methods of deter
25、mination not specified here are known to be capable of achieving equivalent results, but do not conform to this EN (see “Introduction”). Both Method A and Method B are applicable to products having a total lead content greater than or equal to 0,01 %. 2 Normative references The following referenced
26、documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. Publication Year Title EN ISO 1042 1999 Laboratory glassware - One-mark vo
27、lumetric flasks (ISO 1042:1998) EN ISO 3696 1995 Water for analytical laboratory use - Specification and test methods (ISO 3696:1987) ISO 385-1 1984 Laboratory glassware - Burettes - Part 1: General requirements ISO 5725 Series Accuracy (trueness and precision) of measurement methods and results ISO
28、 6503 1984 Paints and varnishes - Determination of total lead - Flame atomic absorption spectrometric method - 5 - EN 50414:2006 3 Methods of analysis 3.1 General In case of dispute, the decomposition of the material by the dry calcination method and the analysis of the material by the flame excitat
29、ion atomic absorption spectrometry (Method A of this standard) shall be the reference method. Method A has been derived from ISO 6503. 3.2 Method A 3.2.1 Principle The lead content is determined using flame excitation atomic absorption spectrometry following the decomposition of a sample by dry calc
30、ination and acid extraction of the residue. 3.2.2 Reagents During the decomposition and extraction, use only reagents of a recognized analytical quality, and demineralized or distilled water of a purity of at least Grade 3 in accordance with EN ISO 3696. 3.2.2.1 sodium carbonate, anhydrous 3.2.2.2 m
31、agnesium carbonate 3.2.2.3 sulfur 3.2.2.4 sodium sulfide, solution at 10 g/l 3.2.2.5 hydrochloric acid, at approximately 180 g/l 450 ml of concentrated hydrochloric acid (36 %, with a specific gravity of approximately 1,18 g/ml) shall be added to approximately 450 ml of water and shall be made up to
32、 1 000 ml. 3.2.2.6 hydrochloric acid, at approximately 18 g/l 100 ml of hydrochloric acid (made up in 3.2.2.5) shall be added to water, and shall be made up to 1 000 ml. 3.2.2.7 nitric acid, at approximately 315 g/l One volume of concentrated nitric acid (about 65 %, with a specific gravity of appro
33、ximately 1,40 g/ml) shall be added to two volumes of water. 3.2.2.8 lead reference solution, containing 1 g of lead per litre Exactly 1 g of lead shall be dissolved in 30 ml of the nitric acid prepared in 3.2.2.7 and shall be transferred, using a funnel, to a 1 000 ml volumetric flask. Distilled or
34、deionized water shall be used to dilute the solution to the mark and shall be mixed well. 1 ml of this reference solution shall contain 1 mg of lead. NOTE ISO 6503 gives further details for the preparation of this solution. 3.2.2.9 lead reference solution, containing 100 mg of lead per litre This so
35、lution shall be prepared fresh each day of its use. EN 50414:2006 - 6 - 10 ml of the reference solution (see 3.2.2.8) shall be transferred with the aid of a pipette into a 100 ml volumetric flask, and shall be diluted to the mark with hydrochloric acid (see 3.2.2.6) and shall be mixed well. 1 ml of
36、this reference solution shall contain 100 g of lead. 3.2.3 Apparatus Ordinary laboratory apparatus, and 3.2.3.1 silica crucibles, preferably new 3.2.3.2 muffle furnace, at (475 25) C 3.2.3.3 hot plate with thermostatic control 3.2.3.4 desiccator 3.2.4 Sampling Take from the cable a representative sa
37、mple of the material to be tested. The sample shall be cut into small pieces of approximately 0,05 g. 3.2.5 Test procedure 3.2.5.1 Preliminary tests If the composition of the material to be tested is not known, carry out qualitative tests to determine whether antimony is present. If the results of t
38、hese tests confirm the presence of antimony, the extraction shall be carried out as specified in 3.2.5.4.2; if not, use the method described in 3.2.5.4.1. 3.2.5.2 Sample Introduce approximately 1 g of the material to be tested into a pre-weighed silica crucible (see 3.2.3.1). Weigh the sample and cr
39、ucible to the nearest 10 mg and determine the actual sample weight. Repeat these tasks. 3.2.5.3 Calcination Spread 2 g of magnesium carbonate (see 3.2.2.2) on to the sample and introduce the crucible into the muffle furnace (see 3.2.3.2) at ambient temperature. Heat the furnace up to a temperature o
40、f 350 C in approximately 30 min, then increase the furnace temperature up to (475 25) C over 60 min and maintain this temperature until complete calcination has been achieved. Make sure that there is sufficient air supply for oxidation. NOTE 1 Care should be taken to ensure that the contents of the
41、crucible do not ignite. NOTE 2 Three hours should be sufficient to ensure complete calcination. If there is any doubt, an extra period of time should be added. 3.2.5.4 Extraction 3.2.5.4.1 Product not containing antimony If the product does not contain antimony (see 3.2.5.1), proceed as follows. All
42、ow the crucible and its contents to cool in a desiccator. Transfer the crucible and the ashes into a 250 ml beaker, add 100 ml of hydrochloric acid (see 3.2.2.5), heat and keep boiling gently for 15 min on the hot plate (see 3.2.3.3). Allow to digest for a further 15 min on the hot plate. - 7 - EN 5
43、0414:2006 While the solution is hot, filter by decantation through a fine texture filter paper into a 250 ml beaker. The filter paper shall consist of undyed cellulose filter paper of a density of (85 15) g/m2with an ash content of less than 0,1 % and particle retention of at least 4 m or better. Wa
44、sh the filter paper and the residue with hot water collecting the rinsings in the beaker. Cool the beaker and transfer the filtrate and the rinsings into a 250 ml volumetric flask. Dilute to the 250 ml mark with water and mix well. 3.2.5.4.2 Product containing antimony If the product does contain an
45、timony (see 3.2.5.1), proceed as follows. Crush the ash to dust, put it into the crucible and mix it with approximately 10 g of a mixture made of equal portions of sodium carbonate (see 3.2.2.1) and sulfur (see 3.2.2.3). Cover the crucible and heat it over a moderate flame until the smell of sulfur
46、dioxide disappears; this should take from 1 h to 2 h. Cool the crucible and digest the contents with a small quantity of hot water until complete dissolution of the residual sodium carbonate/sulfur mixture. Filter, by transferring the whole residue on to a filter paper and wash the residue with the
47、sodium sulfide solution (see 3.2.2.4). Discard the filtrate. Transfer the filter paper and the residue into a 250 ml beaker. Add 15 ml of nitric acid (see 3.2.2.7), heat to boiling and simmer for 15 min on the hot plate (see 3.2.2.3). Add 100 ml of hydrochloric acid (see 3.2.2.5) and allow to digest
48、 for 30 min, whilst still on the hot plate. While the solution is hot, filter through a fine texture filter paper into a 250 ml beaker. Wash the filter paper and the residue with hot water, collecting the rinsings in the beaker. Cool the beaker and transfer the filtrate and the rinsings into a 250 m
49、l volumetric flask. Dilute to the 250 ml mark with water and mix well. 3.2.5.5 Preparation of the blank test solution Repeat the procedures described in 3.2.5.4.2, but omitting the test sample. 3.2.6 Determination 3.2.6.1 Principle An aspiration of the test solution into an acetylene/air flame is followed by measurement of the absorption of the selected spectral line, emitted by a lead hollow cathode lamp or a lead electrodeless discharge lamp within that has a range including 283,3 nm. 3.2.6.2 Reagents and products During the de
