Test on gases evolved during combustion of materials from cables - Part 3: Measurement of low level of halogen content by ion chromatography

IEC 60754-3:2018 specifies the apparatus and procedure for the measurement of the amount of halogens evolved during the combustion of materials taken from electric or optical fibre cable constructions.
The method specified in this document is intended for the measurement of the content of chlorine (Cl), bromine (Br), fluorine (F) and iodine (I), by using the analytical technique of ion chromatography for analysing an aqueous solution resulting from the gases evolved during the combustion.
The heating (combustion) procedure in this part of IEC 60754 is the same as in IEC 60754-2.
The method is intended for materials with an individual halogen content not exceeding 10 mg/g.
The method specified in this document is intended for the testing of individual components used in a cable construction. The use of this method will enable the verification of requirements which are stated in the appropriate cable specification for individual components of a cable construction.
For reasons of precision, this method is not recommended for detecting values of halogens less than 0,1 mg/g of the sample taken.

Essai sur les gaz émis lors de la combustion des matériaux prélevés sur câbles - Partie 3: Mesure d’une faible teneur en halogène par chromatographie ionique

L’IEC 60754-3:2018 spécifie l’appareillage et la procédure pour la mesure de la quantité d’halogènes émis lors de la combustion des matériaux prélevés sur un câble électrique ou à fibre optique.
La méthode spécifiée dans la présente norme est destinée à mesurer la teneur en chlore (Cl), brome (Br), fluor (F) et iode (I) en utilisant la technique analytique de la chromatographie ionique pour l’analyse d’une solution aqueuse obtenue à partir des gaz dégagés pendant la combustion.
La procédure de chauffage (combustion) dans cette partie de l’IEC 60754 est identique à celle utilisée dans l’IEC 60754-2.
Cette méthode est destinée aux matériaux dont la teneur individuelle en halogène ne dépasse pas 10 mg/g.
La méthode spécifiée dans la présente norme est destinée à l’essai des composants individuels utilisés dans la fabrication d’un câble. L’emploi de cette méthode d’essai permettra de vérifier les exigences indiquées dans la spécification appropriée du câble pour les composants individuels d’un câble.
Pour des raisons de précision, l’utilisation de cette méthode n’est pas recommandée pour détecter des valeurs d’halogènes inférieures à 0,1 mg/g de l’échantillon prélevé.

General Information

Status
Published
Publication Date
18-Mar-2018
Technical Committee
Current Stage
PPUB - Publication issued
Start Date
19-Mar-2018
Completion Date
19-Mar-2018
Ref Project

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IEC 60754-3
Edition 1.0 2018-03
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
Test on gases evolved during combustion of materials from cables –
Part 3: Measurement of low level of halogen content by ion chromatography
Essai sur les gaz émis lors de la combustion des matériaux prélevés sur
câbles –
Partie 3: Mesure d’une faible teneur en halogène par chromatographie ionique
IEC 60754-3:2018-03(en-fr)
---------------------- Page: 1 ----------------------
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---------------------- Page: 2 ----------------------
IEC 60754-3
Edition 1.0 2018-03
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
Test on gases evolved during combustion of materials from cables –
Part 3: Measurement of low level of halogen content by ion chromatography
Essai sur les gaz émis lors de la combustion des matériaux prélevés sur
câbles –
Partie 3: Mesure d’une faible teneur en halogène par chromatographie ionique
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
INTERNATIONALE
ICS 13.220.40; 29.060.20 ISBN 978-2-8322-6167-5

Warning! Make sure that you obtained this publication from an authorized distributor.

Attention! Veuillez vous assurer que vous avez obtenu cette publication via un distributeur agréé.

® Registered trademark of the International Electrotechnical Commission
Marque déposée de la Commission Electrotechnique Internationale
---------------------- Page: 3 ----------------------
– 2 – IEC 60754-3:2018 © IEC 2018
CONTENTS

FOREWORD ........................................................................................................................... 4

INTRODUCTION ..................................................................................................................... 6

1 Scope .............................................................................................................................. 7

2 Normative references ...................................................................................................... 7

3 Terms and definitions ...................................................................................................... 7

4 Test method principle ...................................................................................................... 8

5 Test apparatus ................................................................................................................ 8

5.1 General ................................................................................................................... 8

5.2 Tube furnace .......................................................................................................... 8

5.3 Quartz glass tube .................................................................................................... 9

5.4 Combustion boat ..................................................................................................... 9

5.5 Bubbling devices for gases ..................................................................................... 9

5.6 Air supply system .................................................................................................. 10

5.7 Analytical balance ................................................................................................. 10

5.8 Laboratory glassware ............................................................................................ 10

5.9 Ion chromatographic system ................................................................................. 11

6 Test specimen ............................................................................................................... 11

6.1 General ................................................................................................................. 11

6.2 Conditioning of specimen ...................................................................................... 11

6.3 Mass of specimen ................................................................................................. 11

7 Test procedure .............................................................................................................. 11

7.1 General ................................................................................................................. 11

7.2 Blank test .............................................................................................................. 12

7.3 Test apparatus and arrangement .......................................................................... 12

7.4 Heating procedure ................................................................................................ 12

7.5 Washing procedure ............................................................................................... 12

7.6 Measurement of the halogens ............................................................................... 12

8 Evaluation of the test results ......................................................................................... 13

9 Performance requirement .............................................................................................. 13

10 Test report ..................................................................................................................... 13

Annex A (informative) Recommended use and performance requirements ........................... 20

A.1 Recommended use ............................................................................................... 20

A.1.1 General ......................................................................................................... 20

A.1.2 Recommended use of IEC 60754-1, IEC 60754-2 and IEC 60754-3 ............... 21

A.2 Recommended performance requirements to assess materials described as

"halogen free" ....................................................................................................... 21

Bibliography .......................................................................................................................... 22

Figure 1 – Device for inserting combustion boat and test specimen ...................................... 14

Figure 2 – Example of a gas washing bottle .......................................................................... 15

Figure 3 – Test apparatus: method 1 – Use of synthetic or compressed air from a bottle ...... 16

Figure 4 – Test apparatus: method 2 – Use of laboratory compressed air supply .................. 17

Figure 5 – Test apparatus: method 3 – Use of ambient air sucked by means of a

suction pump ........................................................................................................................ 18

---------------------- Page: 4 ----------------------
IEC 60754-3:2018 © IEC 2018 – 3 –

Figure 6 – Example of ion chromatographic system .............................................................. 19

Table A.1 – Scope and recommended use of IEC 60754-1, IEC 60754-2 and

IEC 60754-3 ......................................................................................................................... 21

Table A.2 – Recommended performance requirements to assess materials described

as "halogen free" .................................................................................................................. 21

---------------------- Page: 5 ----------------------
– 4 – IEC 60754-3:2018 © IEC 2018
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
TEST ON GASES EVOLVED DURING
COMBUSTION OF MATERIALS FROM CABLES –
Part 3: Measurement of low level of halogen
content by ion chromatography
FOREWORD

1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising

all national electrotechnical committees (IEC National Committees). The object of IEC is to promote

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8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is

indispensable for the correct application of this publication.

9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of

patent rights. IEC shall not be held responsible for identifying any or all such patent rights.

International Standard IEC 60754-3 has been prepared by IEC technical committee 20:

Electric cables.

This bilingual version (2018-11) corresponds to the monolingual English version, published in

2018-03.
The text of this International Standard is based on the following documents:
FDIS Report on voting
20/1784/FDIS 20/1791/RVD

Full information on the voting for the approval of this International Standard can be found in

the report on voting indicated in the above table.
---------------------- Page: 6 ----------------------
IEC 60754-3:2018 © IEC 2018 – 5 –
The French version of this standard has not been voted upon.

This document has been drafted in accordance with the ISO/IEC Directives, Part 2.

A list of all the parts in the IEC 60754 series, published under the general title Test on gases

evolved during combustion of materials from cables, can be found on the IEC website.

The committee has decided that the contents of this document will remain unchanged until the

stability date indicated on the IEC website under "http://webstore.iec.ch" in the data related to

the specific document. At this date, the document will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.
---------------------- Page: 7 ----------------------
– 6 – IEC 60754-3:2018 © IEC 2018
INTRODUCTION

IEC 60754 consists of the following parts, under the general title: Test on gases evolved

during combustion of materials from cables:
– Part 1: Determination of the halogen acid gas content
– Part 2: Determination of acidity (by pH measurement) and conductivity
– Part 3: Measurement of low level of halogen content by ion chromatography
NOTE Guidance on the corrosivity of fire effluent is given in IEC 60695-5-1.

IEC 60754-1 and IEC 60754-2 were developed due to concerns expressed by cable users

over the amount of acid gas which is evolved when some cable insulating, sheathing and

other materials are burned, as this acid and such corrosive effluents can cause extensive

damage to electrical and electronic equipment not involved in the fire itself.

IEC 60754-1 provides a method for determining the amount of acid gases evolved by burning

cable components so that limits can be agreed for cable specifications.

IEC 60754-2 provides a method for determining the acidity (by pH measurement) and

conductivity of an aqueous solution of gases evolved during the combustion of materials so

that limits can be agreed for cable specifications

IEC 60754-1 is not able to determine hydrofluoric acid and, for reasons of precision, this

method is not recommended for reporting values of halogen acid evolved less than 5 mg/g of

the sample taken.

This document provides a method for measurement of low level of halogen content of the

gases evolved by burning cable and has a high accuracy in the low range of concentration.

The ion chromatic system has an inherently high accuracy. However, the overall accuracy of

the test method is limited by other factors (see Annex A for further information).

This part of IEC 60754 is linked with IEC 60754-2, using the same test procedure for

obtaining the absorption solution.
---------------------- Page: 8 ----------------------
IEC 60754-3:2018 © IEC 2018 – 7 –
TEST ON GASES EVOLVED DURING
COMBUSTION OF MATERIALS FROM CABLES –
Part 3: Measurement of low level of halogen
content by ion chromatography
1 Scope

This part of IEC 60754 specifies the apparatus and procedure for the measurement of the

amount of halogens evolved during the combustion of materials taken from electric or optical

fibre cable constructions.

The method specified in this document is intended for the measurement of the content of

chlorine (Cl), bromine (Br), fluorine (F) and iodine (I), by using the analytical technique of ion

chromatography for analysing an aqueous solution resulting from the gases evolved during

the combustion.

The heating (combustion) procedure in this part of IEC 60754 is the same as in IEC 60754-2.

The method is intended for materials with an individual halogen content not exceeding

10 mg/g.

The method specified in this document is intended for the testing of individual components

used in a cable construction. The use of this method will enable the verification of

requirements which are stated in the appropriate cable specification for individual components

of a cable construction.

NOTE 1 The relevant cable standard indicates which components of the cable are tested.

NOTE 2 This test method is sometimes used to test materials to be used in cable manufacture.

For reasons of precision, this method is not recommended for detecting values of halogens

less than 0,1 mg/g of the sample taken.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their

content constitutes requirements 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.
ISO 1042, Laboratory glassware – One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use – Specification and test methods

ISO 10304-1, Water quality – Determination of dissolved anions by liquid chromatography of

ions – Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and

sulfate
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
---------------------- Page: 9 ----------------------
– 8 – IEC 60754-3:2018 © IEC 2018

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addresses:
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• ISO Online browsing platform: available at http://www.iso.org/obp
3.1
halogen

element of periodic table group 17, specifically fluorine, chlorine, bromine, iodine

3.2
individual halogen content

amount of a halogen in a test specimen that can be converted to water soluble halide ion in

the gaseous combustion effluent from the test specimen
Note 1 to entry: Halide ions are fluoride, chloride, bromide or iodide.

Note 2 to entry: The halogen in the test specimen may be in the form of organic or inorganic compounds.

Note 3 to entry: The individual halogen content is expressed as milligrams of halogen per gram of test specimen.

Note 4 to entry: Halide ions in any solid combustion residue that remains in the combustion boat are not

measured by this test method.
4 Test method principle

The material under test shall be heated in a stream of dry air. The evolved gases shall be

trapped by bubbling through wash bottles filled with distilled or demineralized water.

Each individual halogen content of the resulting solution shall then be determined by using ion

chromatography (IC).

The ion chromatography analysis can be done off line and does not have to be in line.

5 Test apparatus
5.1 General
The apparatus is shown in Figure 1 to Figure 5.

The assembly of the components which constitute the test apparatus shall be leak-tight. The

connecting distances between the quartz glass tube and the first bottle and between

subsequent bottles shall be as short as possible. Quartz glass or polypropylene tubing shall

be used for these connections, unless it is not required to measure and report fluorine, in

which case glass or silicone rubber may be used.

At the exit side of the quartz glass tube, as close to the end as possible, it is permitted to

place a plug of silica wool to aid collection of condensates.

A third empty bottle, of the same size as the gas washing bottles, placed before the gas

washing bottles may be used to improve safety, i.e. to prevent suck-back of water into the

quartz glass tube.
5.2 Tube furnace

The length of the heating zone of the furnace shall be within the range 480 mm to 620 mm

and its inside diameter shall be within the range 38 mm to 62 mm. It shall be equipped with an

adjustable electrical heating system.
---------------------- Page: 10 ----------------------
IEC 60754-3:2018 © IEC 2018 – 9 –
5.3 Quartz glass tube

For the test, a quartz glass tube shall be introduced into the tube furnace. The tube shall be

approximately concentric to the furnace. It shall be resistant to the action of corrosive gases.

The inside diameter of the tube shall be within the range 30 mm to 46 mm. The tube shall

protrude on the entrance side of the furnace by a length of between 60 mm to 200 mm, and

on the exit side by between 60 mm to 100 mm. The initial clearance shall allow for thermal

expansion. For the purposes of measurement of the protrusion distances, the tube shall be

regarded as that part of essentially constant diameter.

The outer diameter of the tube should be chosen with due regard to the inside diameter of the

tube furnace.

Prior to each test, the tube shall be cleaned throughout its length by being calcined at

approximately 950 °C.
5.4 Combustion boat

The combustion boat shall be made of porcelain, fused quartz or soapstone. In case the

method is used to report fluorine, the combustion boat shall be made of quartz glass. The

combustion boat shall have the following dimensions:
– external length: within the range 45 mm to 100 mm;
– external width: within the range 12 mm to 30 mm;
– internal depth: within the range 5 mm to 10 mm.

The dimensions of the boat should be chosen with due regard to the inside diameter of the

quartz tube.

The preferred method for insertion of the combustion boat into the quartz glass tube is shown

in Figure 1.

Prior to each test, the combustion boat shall be washed and calcined in a muffle furnace at

approximately 950 °C for 4 h, after which it shall be introduced into a desiccator and cooled to

ambient temperature. The combustion boat shall then be weighed with a precision of

≤ 0,1 mg until two identical consecutive weights are obtained. This weight m shall be

recorded.
5.5 Bubbling devices for gases

At the exit of the quartz glass tube, the evolved gases shall be trapped by bubbling through

two wash bottles (see Figure 2), each containing approximately 450 ml of distilled or

demineralized water of a purity at least Grade 3 in accordance with ISO 3696.

The wash bottles shall be made of quartz glass, unless it is not required to measure and

report fluorine, in which case wash bottles made of glass may be used.

The pH value of the water shall be between 5,5 and 7,5, and the conductivity less than

0,5 µS/mm.

A magnetic stirrer shall be introduced in the first wash bottle, to get a good swirling motion

and an effective absorption of the combustion gases. The tubes into the wash bottles shall

have a maximum internal diameter at their tip of 5 mm, in order to aid absorption.

The height of the liquid above the end of the tube shall be (110 ± 10) mm in each bottle.

NOTE Use of a wash bottle of internal diameter approximately 75 mm will enable this requirement to be met.

---------------------- Page: 11 ----------------------
– 10 – IEC 60754-3:2018 © IEC 2018
5.6 Air supply system
The gas used for combustion shall be air.

The flow rate of air, ρ, shall be 20 m/h x (π/4) x D with a tolerance of ± 10 %, where D is the

internal diameter of the quartz tube.
EXAMPLES

If D = 30 mm, 20 m/h × (π/4) × D = 14,1 l/h, and the flow rate can be in the range 12,7 l/h to 15,5 l/h.

If D = 46 mm, 20 m/h × (π/4) × D = 33,2 l/h, and the flow rate can be in the range 29,9 l/h to 36,5 l/h.

NOTE The flow rate of air, ρ, is related to the velocity, v, according to the formula

π D
[1]
ρ= v×
where
D is the internal diameter of the tube (mm);
ρ is the flow rate of air (ml/h);
v is the speed of air (ml/mm /h).
If v = 20 m/h, this becomes, ρ = 15,7 m/h × D

The air supply shall be adjusted and controlled by a needle valve, and the flow rate monitored

by a flowmeter of the appropriate range.
The air supplied shall be selected from one of the following methods:
Method 1

This method uses synthetic air or compressed air from a bottle. The air shall be introduced on

the inlet side of the quartz glass tube (see Figure 3).
Method 2

This method uses a laboratory compressed air supply. The air shall be filtered and dried and

shall be introduced on the inlet side of the quartz glass tube (see Figure 4).
Method 3

This method uses the ambient air of the laboratory. The air shall be filtered and dried. In this

case, the mixture of air and combustion gas shall be sucked by a pump (see Figure 5).

5.7 Analytical balance
The balance shall have a precision of ± 0,1 mg or better.
5.8 Laboratory glassware
The following laboratory glassware shall be available:

– one mark volumetric flask in accordance with ISO 1042 class B with 1 000 ml capacity.

The volumetric flask shall be made of quartz glass or polypropylene, unless it is not required

to measure and report fluorine, in which case a volumetric flask made of glass may be used.

---------------------- Page: 12 ----------------------
IEC 60754-3:2018 © IEC 2018 – 11 –
5.9 Ion chromatographic system

In general, the ion chromatographic system consists of the following components (see

Figure 6):
– eluent reservoir;
– IC pump;

– sample injection system, incorporating a sample loop of appropriate volume (e.g. 0,02 ml)

or auto sample device;
– precolumn or guard column;
– separation column;
– suppressor;
– conductivity detector.
6 Test specimen
6.1 General
Two test specimens, each consisting of (1
...

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