EN 61619:1997
(Main)Insulating liquids - Contamination by polychlorinated biphenyls (PCBs) - Method of determination by capillary column gas chromatography
Insulating liquids - Contamination by polychlorinated biphenyls (PCBs) - Method of determination by capillary column gas chromatography
Specifies a method for the determination of polychlorinated biphenyl (PCB) concentration in non-halogenated insulating liquids by high-resolution capillary column gas chromatography using an electron capture detector (ECD). Gives total PCB content; especially useful when a detailed analysis of PCB congeners is necessary.
Isolierflüssigkeiten - Verunreinigung durch polychlorierte Biphenyle (PCBs) - Verfahren zur Bestimmung mittels Kapillar-Gaschromatographie
Isolants liquides - Contamination par les polychlorobiphényles (PCB) - Méthode de détermination par chromatographie en phase gazeuse sur colonne capillaire
Spécifie une méthode de détermination de la concentration des polychorobiphényles (PCB) dans les liquides isolant non halogénés, par chromatographie en phase gazeuse sur colonne capillaire à haute résolution utlisant un détecteur à capture d'électrons (ECD). Donne la teneur totale en PCB et est particulièrement utile quand une analyse détaillée des conénères des PCB est nécessaire.
Insulating liquids - Contamination by polychlorinated biphenyls (PCBs) - Method of determination by capillary column chromatography (IEC 61619:1997)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-november-1998
Insulating liquids - Contamination by polychlorinated biphenyls (PCBs) - Method
of determination by capillary column chromatography (IEC 61619:1997)
Insulating liquids - Contamination by polychlorinated biphenyls (PCBs) - Method of
determination by capillary column gas chromatography
Isolierflüssigkeiten - Verunreinigung durch polychlorierte Biphenyle (PCBs) - Verfahren
zur Bestimmung mittels Kapillar-Gaschromatographie
Isolants liquides - Contamination par les polychlorobiphényles (PCB) - Méthode de
détermination par chromatographie en phase gazeuse sur colonne capillaire
Ta slovenski standard je istoveten z: EN 61619:1997
ICS:
29.040.10 Izolacijska olja Insulating oils
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
NORME
CEI
INTERNATIONALE
IEC
INTERNATIONAL
Première édition
STANDARD
First edition
1997-04
Isolants liquides –
Contamination par les polychlorobiphényles (PCB) –
Méthode de détermination par chromatographie
en phase gazeuse sur colonne capillaire
Insulating liquids –
Contamination by polychlorinated biphenyls (PCBs) –
Method of determination by capillary column gas
chromatography
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Commission Electrotechnique Internationale
PRICE CODE V
International Electrotechnical Commission
Pour prix, voir catalogue en vigueur
For price, see current catalogue
61619 © IEC: 1997 – 3 –
CONTENTS
Page
FOREWORD . 5
Clause
1 Scope and object. 7
2 Normative reference. 7
3 Definitions. 7
4 Principle. 9
5 Reagents and auxiliary materials . 9
6 Apparatus . 13
7 Sample . 17
8 Chromatograph operating conditions . 17
9 Data-processing system . 19
10 Checks of instrumental performance. 21
11 Procedure . 25
12 Test report . 35
13 Detection limit . 35
14 Precision. 37
Annexes
A Test mixtures . 39
B General informations . 53
C Bibliography . 62
61619 © IEC: 1997 – 5 –
INTERNATIONAL ELECTROTECHNICAL COMMISSION
––––––––
INSULATING LIQUIDS –
CONTAMINATION BY POLYCHLORINATED BIPHENYLS (PCBs) –
METHOD OF DETERMINATION BY
CAPILLARY COLUMN GAS CHROMATOGRAPHY
FOREWORD
1) The IEC (International Electrotechnical Commission) is a worldwide organization for standardization comprising
all national electrotechnical committees (IEC National Committees). The object of the IEC is to promote
international co-operation on all questions concerning standardization in the electrical and electronic fields. To
this end and in addition to other activities, the IEC publishes International Standards. Their preparation is
entrusted to technical committees; any IEC National Committee interested in the subject dealt with may
participate in this preparatory work. International, governmental and non-governmental organizations liaising
with the IEC also participate in this preparation. The IEC collaborates closely with the International Organization
for Standardization (ISO) in accordance with conditions determined by agreement between the two
organizations.
2) The formal decisions or agreements of the IEC on technical matters express, as nearly as possible, an
international consensus of opinion on the relevant subjects since each technical committee has representation
from all interested National Committees.
3) The documents produced have the form of recommendations for international use and are published in the form
of standards, technical reports or guides and they are accepted by the National Committees in that sense.
4) In order to promote international unification, IEC National Committees undertake to apply IEC International
Standards transparently to the maximum extent possible in their national and regional standards. Any
divergence between the IEC Standard and the corresponding national or regional standard shall be clearly
indicated in the latter.
5) The IEC provides no marking procedure to indicate its approval and cannot be rendered responsible for any
equipment declared to be in conformity with one of its standards.
6) Attention is drawn to the possibility that some of the elements of this International Standard may be the subject
of patent rights. The IEC shall not be held responsible for identifying any or all such patent rights.
International Standard IEC 61619 has been prepared by technical committee 10: Fluids for
electrotechnical applications.
The text of this standard is based on the following documents:
FDIS Report on voting
10/379/FDIS 10/408/RVD
Full information on the voting for the approval of this standard can be found in the report on
voting indicated in the above table.
Annex A forms an integral part of this standard.
Annexes B and C are for information only.
61619 © IEC: 1997 – 7 –
INSULATING LIQUIDS –
CONTAMINATION BY POLYCHLORINATED BIPHENYLS (PCBs) –
METHOD OF DETERMINATION BY
CAPILLARY COLUMN GAS CHROMATOGRAPHY
1 Scope and object
This International Standard specifies a method for the determination of polychlorinated
biphenyl (PCB) concentration in non-halogenated insulating liquids by high-resolution capillary
column gas chromatography using an electron capture detector (ECD).
The method gives the total PCB content and is especially useful when a detailed analysis of
PCB congeners is necessary. Other methods, such as IEC 60997, may be used when a less
detailed analysis is acceptable.
The method is applicable to unused, reclaimed (including dechlorinated and chemically and/or
physically treated), or used insulating liquids contaminated by PCBs.
2 Normative reference
The following normative document contains provisions which, through reference in this text,
constitute provisions of this normative document. At the time of publication, the edition
indicated was valid. All normative documents 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 normative document indicated below. Members of IEC and ISO
maintain registers of current valid International Standards.
IEC 60475: 1974, Method of sampling liquid dielectrics
3 Definitions
For the purposes of the International Standard, the following definitions apply:
3.1 Polychlorinated biphenyl (PCB)
A biphenyl substituted by one to ten chlorine atoms.
NOTE – For legal purposes, congeners with one, two or ten chlorine atoms may be excluded from this definition.
3.2 Congener
All the chlorine derivatives of biphenyl, irrespective of the number of chlorine atoms, are
termed congeners.
*
NOTE – There are 209 possible PCB congeners.These are listed in table B.1. The congener numbers (IUPAC)
are for easy identification; they do not represent the order of chromatographic elution.
––––––––––
*
International Union of Pure and Applied Chemistry.
61619 © IEC: 1997 – 9 –
4 Principle
The PCB congeners are determined by temperature programmed gas chromatography. The
chromatograph uses a high-efficiency capillary column to separate the PCBs into single or
small groups of overlapping congeners.
The sensitivity of the electron capture detector (ECD) may be reduced by the presence of
mineral oil. In this method the sample is diluted 100 times to reduce this effect to a minimum.
A sample preparation (clean-up) procedure is used to remove most of the impurities likely to
interfere with the determination.
Reference compounds are included to enable calculation of experimental relative retention
times (ERRTs) which are compared to a data file of peak ERRTs to identify individual or groups
of unresolved congeners. An internal standard is added for quantification.
Relative response factors (RRF), taken from the data files (9.1), corrected by experimental
relative response factors (ERRFs) obtained from reference compounds, are applied to
identified peaks to quantify the individual (or groups of) congeners, and the values summed to
give total PCB content.
5 Reagents and auxiliary materials
5.1 Reagents and standards
All reagents and materials, including those for clean-up, shall be free from PCB contamination
and compounds responding to the ECD.
5.1.1 Solvent
Hexane, heptane, cyclohexane or isooctane (2,2,4-trimethylpentane), high purity, free from
PCB contamination and low in compounds that respond to the ECD.
5.1.2 Hexachlorobenzene
Purity 99 % at least, used for checking detector sensitivity.
5.1.3 Insulating liquid
An insulating liquid, checked to be free from PCBs or other interfering substances, of the same
type as is present in the sample.
5.1.4 Congener 30 solution (C 30)
10 mg/l in solvent (5.1.1) purchased in solution or prepared from pure material (purity 99 % at
least).
5.1.5 Congener 209 (DCB), decachlorobiphenyl solution
10 mg/l in solvent (5.1.1) purchased in solution or prepared from pure material (purity 99% at
least).
61619 © IEC: 1997 – 11 –
5.1.6 Calibration solution of selected PCB congeners
Certified calibration mixture in solvent (5.1.1) containing at least the following PCB congeners
at a concentration of 10 mg/l each: 18, 28, 31, 44, 52, 101, 118, 138, 149, 153, 170, 180, 194
and 209 (see B.3).
5.2 Commercial PCB standards (see B.4)
5.2.1 Solutions of Aroclors 1242, 1254 and 1260 in solvent (5.1.1)
Concentration required 50 mg/l or more, typically 1000 mg/l.
5.2.2 Solutions of Aroclors 1242, 1254 and 1260 in oil
50 mg/kg solutions of Aroclors 1242, 1254 and 1260 in unused insulating liquid, either
purchased as standardized solutions or prepared from pure material.
5.3 Gas chromatography gases
5.3.1 Carrier gas: helium or hydrogen, purity 99,99 % at least.
5.3.2 Make-up gas: argon/methane, 95% 5%. Alternatively, 99,99 % minimum purity
nitrogen can be used.
5.4 Internal standard/reference solutions
NOTE – Standards should be stored in a cool, dark place.
5.4.1 Internal standard solution 2 (IS 2)
2 mg/l C209 (DCB), 2 mg/l C30.
Pipette (5.8.3) 5 ml of DCB solution (5.1.5) and 5 ml C30 solution (5.1.4) into a 25 ml
volumetric flask, make up to the mark with solvent (5.1.1).
5.4.2 Internal standard solution 0,5 (IS 0,5)
0,5 mg/l C209 (DCB), 0,5 mg/l C30.
Follow 5.4.1 using a 100 ml volumetric flask.
5.5 Test mixture solution (for system evaluation)
Into a 20 ml volumetric flask: weigh, to the nearest 0,001 g, 0,50 g of 50 mg/kg Aroclor 1260,
plus 0,50 g of 50 mg/kg Aroclor 1254 plus 1,00 g of 50 mg/kg Aroclor 1242 solutions in
insulating liquid (5.2.2).
Add by pipette 1 ml of IS 2 solution (5.4.1) and make up to volume with solvent.
Prior to use this solution shall be treated as per 11.1.3.
5.6 Calibration – congener mix stock solution
Into a 20 ml volumetric flask: weigh, to the nearest 0,001 g, 2,0 g of insulating liquid (5.1.3) and
add 1 ml of the calibration PCB congener mix (5.1.6). Make up to the mark with solvent (5.1.1).
61619 © IEC: 1997 – 13 –
5.7 Congener mix calibration solution (for response factors)
Submit 500 μl of solution (5.6) to the clean-up (11.1.3). The final solution is suitable for the
determination of relative factors.
Prepare a fresh solution monthly.
5.8 Glassware
5.8.1 Volumetric flasks 100, 50, 25, 10 and 5 ml (tolerance better than ± 0,4%)
5.8.2 Syringes and pipettes:
500 μl ± 5 μl syringe or pipette,
1 μl and 5 μl gas chromatography precision syringes.
5.8.3 Bulb pipettes (volumetric) 1, 2 and 5 ml class A
5.9 Columns and accessories for sample preparation
5.9.1 Commercial or self-packed solid-phase extraction columns:
3 ml silica gel column, adsorbent weight 500 mg, particle size 40 μm,
3 ml benzenesulphonic acid column, adsorbent weight 500 mg, particle size 40 μm.
5.9.2 Column adapter, for joining two columns
5.9.3 Vacuum manifold column processor – optional
6 Apparatus
6.1 Gas chromatograph (GC)
A high-resolution gas chromatograph with accurately reproducible oven temperature control,
capable, when used with the appropriate column and conditions, of resolving the test mixture
(5.5) at least as well as in figure A.1 (90 peaks observed) and of reproducing relative retention
times to within ± 0,0015.
The gas lines (carrier gas and make-up gas) shall be fitted with water vapour and oxygen traps.
The carrier gas supply system shall be capab
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