IEC 60666:2010

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.

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.

General Information

• Status: Published
• Publication Date: 25-Apr-2010
• ICS: 01 - GENERALITIES. TERMINOLOGY. STANDARDIZATION. DOCUMENTATION
• ICS: 17.220.99 - Other standards related to electricity and magnetism
• ICS: 29.040.10 - Insulating oils
• Technical Committee: TC 10 - Fluids for electrotechnical applications
• Current Stage: PPUB - Publication issued
• Start Date: 30-Apr-2010
• Completion Date: 26-Apr-2010

Standards Content (Sample)

IEC 60666 ®
Edition 2.0 2010-04
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
colour
inside
Detection and determination of specified additives in mineral insulating oils

Détection et dosage d’additifs spécifiques présents dans les huiles minérales
isolantes
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IEC 60666 ®
Edition 2.0 2010-04
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
colour
inside
Detection 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
PRICE CODE
INTERNATIONALE
V
CODE PRIX
ICS 17.220.99, 29.040.10 ISBN 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).
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

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
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