IEC 60666:2010

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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