Detection and determination of specified additives in mineral insulating oils

IEC 60666:2010 provides methods concerning the detection and determination of specified additives in unused and used mineral insulating oils. The detection methods may be applied to assess whether or not a mineral insulating oil contains an additive as specified by the supplier. The determination methods are used for the quantitative determination of additives known to be present or previously detected by the appropriate detection method. The main changes with respect to the previous edition are listed below: - a change in the title from 'Detection and determination of specified anti-oxidant additives in insulating oils'; - new Annexes B and C which provide methods for the determination of two additives different from the anti-oxidants.

Nachweis und Bestimmung spezifizierter Additive in Isolierflüssigkeiten auf Mineralölbasis

Détection et dosage d'additifs spécifiques présents dans les huiles minérales isolantes

La CEI 60666:2010 fournit des méthodes concernant la détection et le dosage d'additifs spécifiques dans les huiles minérales isolantes neuves et usagées. Les méthodes de détection peuvent être appliquées pour vérifier si une huile isolante minérale contient ou non un additif comme le déclare le fournisseur. Les méthodes de dosage sont utilisées pour le dosage quantitatif des additifs préalablement décelés par la méthode de détection appropriée. Les modifications principales par rapport à l'édition précédente sont les suivantes: - un changement dans le titre de ' Détection et dosage d'additifs antioxydants spécifiques présents dans les huiles isolantes '; - les nouvelles Annexes B et C, qui donnent des méthodes pour la détermination de deux additifs différents de l'anti-oxydant.

Odkrivanje in ugotavljanje specifičnih aditivov v mineralnih izolacijskih oljih (IEC 60666:2010)

Metode, opisane v tem mednarodnem standardu, se nanašajo na odkrivanje in ugotavljanje specifičnih aditivov v neuporabljenih in uporabljenih mineralnih izolacijskih oljih. Metode odkrivanja se lahko uporabijo za ocenjevanje, ali mineralno izolacijsko olje vsebuje aditiv, ki ga navaja proizvajalec. Metode ugotavljanja se uporabljajo za količinsko določevanje aditivov, za katere je znano, da so prisotni, ali ki so bili predhodno odkriti z ustrezno metodo odkrivanja.

General Information

Status
Published
Publication Date
08-Jul-2010
Withdrawal Date
30-Jun-2013
Current Stage
6060 - Document made available - Publishing
Completion Date
09-Jul-2010

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Nachweis und Bestimmung spezifizierter Additive in Isolierflüssigkeiten auf Mineralölbasis (IEC 60666:2010)Détection et dosage d'additifs spécifiques présents dans les huiles minérales isolantes (CEI 60666:2010)Detection and determination of specified additives in mineral insulating oils (IEC 60666:2010)29.040.10Izolacijska oljaInsulating oilsICS:Ta slovenski standard je istoveten z:EN 60666:2010SIST EN 60666:2010en01-september-2010SIST EN 60666:2010SLOVENSKI
STANDARDSIST HD 415 S1:19991DGRPHãþD

EUROPEAN STANDARD EN 60666 NORME EUROPÉENNE
EUROPÄISCHE NORM July 2010
CENELEC European Committee for Electrotechnical Standardization Comité Européen de Normalisation Electrotechnique Europäisches Komitee für Elektrotechnische Normung
Management Centre: Avenue Marnix 17, B - 1000 Brussels
© 2010 CENELEC -
All rights of exploitation in any form and by any means reserved worldwide for CENELEC members.
Ref. No. EN 60666:2010 E
ICS 17.220.99; 29.040.10 Supersedes HD 415 S1:1981
English version
Detection and determination of specified additives
in mineral insulating oils (IEC 60666:2010)
Détection et dosage d'additifs spécifiques présents dans les huiles minérales isolantes (CEI 60666:2010)
Nachweis und Bestimmung spezifizierter Additive in Isolierflüssigkeiten
auf Mineralölbasis (IEC 60666:2010)
This European Standard was approved by CENELEC on 2010-07-01. 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, Bulgaria, Croatia, 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.
at national level by publication of an identical
national standard or by endorsement
(dop)
2011-04-01 – latest date by which the national standards conflicting
with the EN have to be withdrawn
(dow)
2013-07-01 Annex ZA has been added by CENELEC. __________ Endorsement notice The text of the International Standard IEC 60666:2010 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: [3] IEC 60422 NOTE
Harmonized as EN 60422. [5] IEC 61198 NOTE
Harmonized as EN 61198. __________ SIST EN 60666:2010

- 3 - EN 60666:2010 Annex ZA
(normative)
Normative references to international publications with their corresponding European publications
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.
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 60296 - Fluids for electrotechnical applications - Unused mineral insulating oils for transformers and switchgear EN 60296 -
IEC 60475 - Method of sampling liquid dielectrics - -
ISO 5725 Series Accuracy (trueness and precision) of measurement methods and results - -
IEC 60666Edition 2.0 2010-04INTERNATIONAL STANDARD NORME INTERNATIONALEDetection and determination of specified additives in mineral insulating oils
Détection et dosage d’additifs spécifiques présents dans les huiles minérales isolantes
INTERNATIONAL ELECTROTECHNICAL COMMISSION COMMISSION ELECTROTECHNIQUE INTERNATIONALE VICS 17.220.99, 29.040.10 PRICE CODECODE PRIXISBN 978-2-88910-244-0
– 2 – 60666 © IEC:2010 CONTENTS FOREWORD.4 INTRODUCTION.6 1 Scope.7 2 Normative references.7 3 Methods for the determination of anti-oxidant additives.7 3.1 Determination of phenolic and amine-based antioxidants by infrared (IR) spectrophotometry – Method A.7 3.1.1 Introductory remark.7 3.1.2 Equipment, materials and solvents.8 3.1.3 Sample preparation.8 3.1.4 Calibration.8 3.1.5 Analysis.9 3.1.6 Calculation.9 3.1.7 Precision.10 3.1.8 Repeatability.10 3.1.9 Reproducibility.10 3.1.10 Report.10 3.2 Determination of 2,6-di-tert-butyl-para-cresol by IR spectrophotometry –
Method B.10 3.2.1 Calibration.11 3.2.2 Sample test – New or used oil.11 3.2.3 Precision.11 3.2.4 Repeatability.11 3.2.5 Reproducibility.11 3.2.6 Report.12 3.3 Determination of 2,6-di-tert-butyl-para-cresol (DBPC) by high performance liquid chromatography (HPLC).12 3.3.1 Introductory remark.12 3.3.2 Materials and equipment.12 3.3.3 Reagents and solvents.12 3.3.4 Solid-liquid extraction.12 3.3.5 Analysis of the extract.12 3.3.6 Calculation.13 3.3.7 Precision.13 3.3.8 Repeatability.13 3.3.9 Reproducibility.13 3.3.10 Report.13 3.4 Determination of phenolic inhibitors by gas chromatography – Mass spectrometry (GC-MS).14 3.4.1 Summary of method.14 3.4.2 Example of instrument parameters.14 3.4.3 GC accessories.14 3.4.4 Calibration standard solutions.14 3.4.5 Internal standard solutions.14 3.4.6 Preparation of samples and calibration standards.15 3.4.7 Analytical procedure.15 3.4.8 Calculation of results.15 3.4.9 Precision.16 SIST EN 60666:2010

60666 © IEC:2010 – 3 –
3.4.10 Report.16 Annex A (informative)
Detection of anti-oxidant additives by thin layer chromatography (TLC).17 Annex B (informative)
Analysis method for determination of passivators in mineral oils by high performance liquid chromatography (HPLC).22 Annex C (informative)
Determination of pour point depressants by gel permeation chromatography.30 Bibliography.32
Figure A.1 – Typical infrared spectrum to determine DBPC content.19 Figure A.2 – Typical infrared spectrum with 0,3 % DBPC.20 Figure A.3 – Typical HPLC chromatogram to determine DBPC content.21 Figure B.1 – UV spectra of TTAA (in blue) and BTA (in red).26
Table B.1 – Examples of separation conditions.26 Table B.2 – Repeatability.29 Table B.3 – Reproducibility.29
– 4 – 60666 © IEC:2010 INTERNATIONAL ELECTROTECHNICAL COMMISSION ____________
DETECTION AND DETERMINATION OF SPECIFIED
ADDITIVES IN MINERAL INSULATING OILS
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 international co-operation on all questions concerning standardization in the electrical and electronic fields. To this end and in addition to other activities, IEC publishes International Standards, Technical Specifications, Technical Reports, Publicly Available Specifications (PAS) and Guides (hereafter referred to as “IEC Publication(s)”). 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. 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 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 IEC National Committees.
3) IEC Publications have the form of recommendations for international use and are accepted by IEC National Committees in that sense. While all reasonable efforts are made to ensure that the technical content
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