SIST EN 50414:2006

SLOVENSKI SIST EN 50414:2006

STANDARD
oct 2006
Preskusne metode za analizo svinca v PVC (polivinilkloridu), ki se uporablja
za izolacijo in oplaščenje električnih kablov in kablov z optičnimi vlakni -
Metoda A: Določevanje celotnega svinca z atomsko absorpcijsko
spektrometrijo z vzbujanjem plamena - Metoda B: Kvalitativna metoda z
barvanjem s svinčevim sulfidom
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
ICS 29.035.20; 29.060.20 Referenčna številka
SIST EN 50414:2006(en)
©  Standard je založil in izdal Slovenski inštitut za standardizacijo. Razmnoževanje ali kopiranje celote ali delov tega dokumenta ni dovoljeno

---------------------- Page: 1 ----------------------

EUROPEAN STANDARD
EN 50414

NORME EUROPÉENNE
April 2006
EUROPÄISCHE NORM

ICS 29.035.20


English version


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


Méthodes d'analyse du plomb  Prüfverfahren für die Analyse von Blei
dans le PVC prélevé de l'enveloppe in PVC entnommen aus Isolierung
isolante et des gaines des câbles und Mantel von Kabeln, isolierten
électriques et à fibres optiques - Leitungen und Lichtwellenleiterkabeln -
Méthode A: Détermination de la teneur Verfahren A: Bestimmung
totale en plomb par spectrométrie des Gesamtbleigehalts mit der Flammen-
atomique d'absorption dans la flamme - Atomabsorptionsspektrometrie -
Méthode B: Analyse qualitative du plomb Verfahren B: Qualitative Analyse
par production de sulfure de plomb des Bleigehalts durch Bleisulfidverfärbung



This European 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 references 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 member 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, Italy, Latvia,
Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.

CENELEC
European Committee for Electrotechnical Standardization
Comité Européen de Normalisation Electrotechnique
Europäisches Komitee für 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

---------------------- Page: 2 ----------------------

EN 50414:2006 - 2 -

Foreword
This European Standard was prepared by the Technical Committee CENELEC TC 20, Electric cables.
The text 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 by which the national standards conflicting
with the EN have to be withdrawn (dow) 2009-03-01
__________

---------------------- Page: 3 ----------------------

- 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 Apparatus.6
3.2.4 Sampling .6
3.2.5 Test procedure .6
3.2.6 Determination .7
3.2.7 Tests results.9
3.2.8 Test report.10
3.3 Method B.10
3.3.1 Principle .10
3.3.2 Reagents.10
3.3.3 Apparatus.10
3.3.4 Procedure.10
3.3.5 Determination .11
3.3.6 Test report.11
Table 1 - Preparation of reference solutions.8

---------------------- Page: 4 ----------------------

EN 50414:2006 - 4 -

Introduction
The 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 uses 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 determination 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 such 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 sheathing
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 determination 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 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 volumetric 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 6503 1984 Paints and varnishes - Determination of total lead - Flame atomic
absorption spectrometric method

---------------------- Page: 5 ----------------------

- 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 excitation 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 calcination 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 magnesium 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 ρ of approximately 1,18 g/ml) shall
be added to approximately 450 ml of water and shall be made up to 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 ρ of approximately 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 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 solution shall be prepared fresh each day of its use.

---------------------- Page: 6 ----------------------

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 this reference solution shall contain 100 µg 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 sample 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 these 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 Sampl
...