EN 62697-1:2012

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno./Méthodes d'essai pour la déterminationquantitative des composés de soufre corrosif dans les liquides isolants usagés et neufs - Partie 1: Méthode d'essaipour la détermination quantitative du disulfure de dibenzyle (DBDS)Test method for quantitative determination of corrosive sulfur compounds in unused and used insulating liquids - Part 1: Test method for quantitative determination of dibenzyldisulfide (DBDS)29.040.01Izolacijski fluidi na splošnoInsulating fluids in generalICS:Ta slovenski standard je istoveten z:EN 62697-1:2012SIST EN 62697-1:2013en01-januar-2013SIST EN 62697-1:2013SLOVENSKI
STANDARD
EUROPEAN STANDARD EN 62697-1 NORME EUROPÉENNE
EUROPÄISCHE NORM November 2012
CENELEC European Committee for Electrotechnical Standardization Comité Européen de Normalisation Electrotechnique Europäisches Komitee für Elektrotechnische Normung
Management Centre: Avenue Marnix 17, B - 1000 Brussels
© 2012 CENELEC -
All rights of exploitation in any form and by any means reserved worldwide for CENELEC members.
Ref. No. EN 62697-1:2012 E
ICS 29.040
English version
Test methods for quantitative determination of corrosive sulfur compounds in unused and used insulating liquids -
Part 1: Test method for quantitative determination
of dibenzyldisulfide (DBDS) (IEC 62697-1:2012)
Méthodes d'essai pour la détermination quantitative des composés de soufre corrosif dans les liquides isolants
usagés et neufs -
Partie 1: Méthode d'essai
pour la détermination quantitative
du disulfure de dibenzyle (DBDS) (CEI 62697-1:2012)
Prüfverfahren zur quantitativen Bestimmung von Verbindungen korrosiven Schwefels in neuen und gebrauchten Isolierflüssigkeiten -
Teil 1: Prüfverfahren zur quantitativen Bestimmung von Dibenzyldisulfid (DBDS)(IEC 62697-1:2012)
This European Standard was approved by CENELEC on 2012-09-28. 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 CEN-CENELEC Management Centre 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 CEN-CENELEC Management Centre has the same status as the official versions.
CENELEC members are the national electrotechnical committees of Austria, Belgium, Bulgaria, Croatia, Cyprus, the Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CENELEC [and/or CEN] shall not be held responsible for identifying any or all such patent rights.
Endorsement notice The text of the International Standard IEC 62697-1:2012 was approved by CENELEC as a European Standard without any modification. In the official version, for Bibliography, the following notes have to be added for the standards indicated:
IEC 60296 NOTE Harmonised as EN 60296. IEC 60422 NOTE Harmonised as EN 60422. IEC 60567 NOTE Harmonised as EN 60567.
- 3 - EN 62697-1:2012 Annex ZA
(normative)
Normative references to international publications with their corresponding European publications
The following documents, in whole 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.
NOTE
When an international publication has been modified by common modifications, indicated by (mod), the relevant EN/HD applies.
Publication Year Title EN/HD Year
IEC 60475 - Method of sampling insulating liquids EN 60475 -
IEC 62535 2008 Insulating liquids - Test method
for detection of potentially corrosive
sulphur in used and unused insulating oil EN 62535 2009
IEC 62697-1 Edition 1.0 2012-08 INTERNATIONAL STANDARD NORME INTERNATIONALE Test methods for quantitative determination of corrosive sulfur compounds in unused and used insulating liquids –
Part 1: Test method for quantitative determination of dibenzyldisulfide (DBDS)
Méthodes d’essai pour la détermination quantitative des composés de soufre corrosif dans les liquides isolants usagés et neufs –
Partie 1: Méthode d’essai pour la détermination quantitative du disulfure de dibenzyle (DBDS)
INTERNATIONAL ELECTROTECHNICAL COMMISSION COMMISSION ELECTROTECHNIQUE INTERNATIONALE V ICS 29.040 PRICE CODE CODE PRIX ISBN 978-2-83220-305-7
– 2 – 62697-1 © IEC:2012 CONTENTS FOREWORD . 5 INTRODUCTION . 7 1 Scope . 9 2 Normative references . 9 3 Terms, definitions and abbreviations . 9 3.1 Terms and definitions . 9 3.2 Abbreviations . 13 4 Sampling . 13 5 Procedure . 13 5.1 Principle . 13 5.2 Significance and use . 13 5.3 Interferences . 14 5.3.1 Co-eluting compounds . 14 5.3.2 Electron capture detector (ECD) . 14 5.3.3 Atomic emission detector (AED) . 14 5.3.4 Mass spectrometer (MS) . 14 5.3.5 MS/MS . 14 5.3.6 Interference from the matrix . 14 5.4 Apparatus . 15 5.4.1 Balance . 15 5.4.2 Gas chromatography system . 15 5.4.3 Data system . 16 5.5 Reagents and materials . 16 5.5.1 Purity of reagents . 16 5.5.2 Gases . 16 5.5.3 Solvents . 16 5.6 Standard materials . 16 5.6.1 Dibenzyl disulfide (DBDS) . 16 5.6.2 Diphenyl disulfide (DPDS) . 16 5.6.3 Blank oil . 16 5.7 Standard solutions . 17 5.7.1 Stock solution . 17 5.7.2 Internal standard (IS) solution. 17 6 Instrument set-up . 17 6.1 Gas chromatograph . 17 6.1.1 General . 17 6.1.2 Carrier gas . 17 6.1.3 Injector . 17 6.1.4 Separation parameters . 17 6.1.5 ECD detection . 18 6.1.6 AED detection . 18 6.1.7 MS detection . 18 6.1.8 MS/MS detection . 18 6.2 Calibration . 19 6.2.1 General . 19 6.2.2 Calibration procedure . 19 SIST EN 62697-1:2013

62697-1 © IEC:2012 – 3 – 6.2.3 Response factor determination (ECD and AED) . 19 6.2.4 Response factor determination (MS) . 19 6.2.5 Response factor determination (MS/MS) . 20 6.3 Analysis . 20 6.3.1 Sample pre-treatment . 20 6.3.2 Sample injection . 20 6.3.3 Chromatographic run . 20 6.3.4 Peak integration . 20 6.4 Calculations . 21 6.4.1 ECD and AED . 21 6.4.2 Mass spectrometer (MS) . 21 6.4.3 MS/MS . 21 6.5 Results . 21 7 Precision data . 21 7.1 Detection limit . 21 7.2 Repeatability . 22 7.3 Reproducibility . 22 8 Report . 22 Annex A (informative)
Figures with typical chromatograms and results . 23 Annex B (informative)
Operating parameters for other suitable detectors . 30 Bibliography . 31
Figure A.1 – GC-ECD chromatogram of 2 mg kg–1 DBDS and DPDS (IS) in white mineral oil . 23 Figure A.2 – GC-ECD chromatogram of 200 mg kg–1 DBDS and DPDS (IS) in white mineral oil . 24 Figure A.3 – GC-ECD chromatogram of commercial mineral insulating oil with a known DBDS contamination . 24 Figure A.4 – GC-ECD chromatogram of commercial mineral insulating oil with no known DBDS contamination .
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