Insulating liquids - Test methods for oxidation stability - Test method for evaluating the oxidation stability of insulating liquids in the delivered state

IEC 61125:2018 describes a test method for evaluating the oxidation stability of insulating liquids in the delivered state under accelerated conditions regardless of whether or not antioxidant additives are present. The duration of the test can be different depending on the insulating liquid type and is defined in the corresponding standards (e.g. in IEC 60296, IEC 61099, IEC 62770). The method can be used for measuring the induction period, the test being continued until the volatile acidity significantly exceeds 0,10 mg KOH/g in the case of mineral oils. This value can be significantly higher in the case of ester liquids.
Additional test methods such as those described in IEC TR 62036 based on differential scanning calorimetry can also be used as screening tests, but are out of the scope of this document.
This second edition cancels and replaces the first edition published in 1992 and Amendment 1: 2004. This edition constitutes a technical revision.
This edition includes the following significant technical changes with respect to the previous edition:
a) the title has been modified to include insulating liquids different from mineral insulating oils (hydrocarbon);
b) the method applies for insulating liquids in the delivered state;
c) former Method C is now the main normative method;
d) precision data of the main normative method has been updated concerning the dissipation factor;
e) former Method A has been deleted;
f) former Method B has been transferred to Annex B;
g) a new method evaluating the thermo-oxidative behaviour of esters is included in Annex C.

Isolants liquides - Méthodes d'essai de la stabilité à l'oxydation - Méthode d’essai pour évaluer la stabilité à l’oxydation des isolants liquides tels que livrés

L'IEC 61125:2018 spécifie une méthode d’essai permettant d’évaluer dans des conditions accélérées la stabilité à l’oxydation des isolants liquides tels que livrés, que des additifs antioxydants soient présents ou non. La durée de l’essai peut différer selon les types d’isolants liquides, et elle est définie dans les normes correspondantes (par exemple, dans l’IEC 60296, l’IEC 61099, l’IEC 62770). La méthode peut être utilisée pour mesurer la période d’induction, l’essai se poursuivant jusqu’à ce que l’acidité volatile dépasse significativement 0,10 mg KOH/g dans le cas des huiles minérales. Cette valeur peut être nettement plus élevée dans le cas des esters liquides.
Des méthodes d’essai complémentaires, par exemple celles basées sur l’analyse calorimétrique différentielle par balayage décrites dans l’IEC TR 62036, peuvent également être utilisées comme test de dépistage, mais elles ne font toutefois pas partie du domaine d’application du présent document.
Cette deuxième édition annule et remplace la première édition parue en 1992 et l’Amendement 1: 2004. Cette édition constitue une révision technique.
Cette édition inclut les modifications techniques majeures suivantes par rapport à l'édition précédente:
a) modification du titre afin d’inclure les isolants liquides différents des huiles minérales isolantes (hydrocarbures);
b) application de la méthode aux isolants liquides tels que livrés;
c) l’ancienne méthode C est dorénavant la méthode normative principale;
d) actualisation des données de fidélité de la méthode normative principale concernant le facteur de dissipation;
e) suppression de l’ancienne méthode A;
f) transfert de l’ancienne méthode B dans l’Annexe B;
g) une nouvelle méthode d'évaluation de la stabilité à l’oxydation thermique des esters est proposée dans l’Annexe C.

General Information

Status
Published
Publication Date
11-Jan-2018
Current Stage
PPUB - Publication issued
Completion Date
12-Jan-2018
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IEC 61125
Edition 2.0 2018-01
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
colour
inside
Insulating liquids – Test methods for oxidation stability
Test method for evaluating the oxidation stability of insulating liquids in the
delivered state
Isolants liquides – Méthodes d’essai de la stabilité à l’oxydation

Méthode d’essai pour évaluer la stabilité à l’oxydation des isolants liquides tels

que livrés
IEC 61125:2018-01(en-fr)
---------------------- Page: 1 ----------------------
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---------------------- Page: 2 ----------------------
IEC 61125
Edition 2.0 2018-01
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
colour
inside
Insulating liquids – Test methods for oxidation stability
Test method for evaluating the oxidation stability of insulating liquids in the
delivered state
Isolants liquides – Méthodes d’essai de la stabilité à l’oxydation

Méthode d’essai pour évaluer la stabilité à l’oxydation des isolants liquides tels

que livrés
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
INTERNATIONALE
ICS 29.040.10 ISBN 978-2-8322-5210-9

Warning! Make sure that you obtained this publication from an authorized distributor.

Attention! Veuillez vous assurer que vous avez obtenu cette publication via un distributeur agréé.

® Registered trademark of the International Electrotechnical Commission
Marque déposée de la Commission Electrotechnique Internationale
---------------------- Page: 3 ----------------------
– 2 – IEC 61125:2018 © IEC 2018
CONTENTS

FOREWORD ........................................................................................................................... 5

1 Scope .............................................................................................................................. 7

2 Normative references ...................................................................................................... 7

3 Terms and definitions ...................................................................................................... 8

4 Apparatus ........................................................................................................................ 9

4.1 General principle of the method .............................................................................. 9

4.2 Equipment .............................................................................................................. 9

4.2.1 Heating arrangement ....................................................................................... 9

4.2.2 Test vessels .................................................................................................. 10

4.2.3 Absorption tubes............................................................................................ 10

4.2.4 Filtering crucibles .......................................................................................... 10

4.2.5 Porcelain vessels........................................................................................... 11

4.2.6 Flowmeter...................................................................................................... 11

4.2.7 Timer ............................................................................................................. 11

4.2.8 Gas supply .................................................................................................... 11

4.2.9 Analytical balance ......................................................................................... 11

4.2.10 Burette .......................................................................................................... 11

4.2.11 Volumetric pipette .......................................................................................... 11

4.2.12 Volumetric flask ............................................................................................. 12

4.2.13 Graduated measuring cylinder ....................................................................... 12

4.2.14 Thermometer ................................................................................................. 12

4.2.15 Erlenmeyer flask ............................................................................................ 12

4.3 Reagents .............................................................................................................. 12

4.3.1 Normal heptane ............................................................................................. 12

4.3.2 Alkali blue 6B indicator according to IEC 62021-2 .......................................... 12

4.3.3 Phenolphthalein indicator .............................................................................. 12

4.3.4 Potassium hydroxide according to IEC 62021-2 ............................................. 12

4.3.5 Oxidant gas ................................................................................................... 12

4.3.6 Acetone ......................................................................................................... 12

4.4 Cleaning of test vessels ........................................................................................ 12

4.5 Catalyst ................................................................................................................ 13

4.6 Insulating liquid sample conditioning ..................................................................... 13

4.7 Preparation of the test .......................................................................................... 13

4.8 Determinations on the oxidized insulating liquid .................................................... 13

4.8.1 Sludge formation ........................................................................................... 13

4.8.2 Soluble acidity (SA) ....................................................................................... 14

4.8.3 Volatile acidity (VA) ....................................................................................... 14

4.8.4 Total acidity (TA) ........................................................................................... 15

4.8.5 Dielectric dissipation factor (DDF) ................................................................. 15

4.8.6 Oxidation rate with air .................................................................................... 15

4.8.7 Induction period with air (IP with air) (optional) .............................................. 15

4.9 Report................................................................................................................... 15

4.10 Precision ............................................................................................................... 16

4.10.1 General ......................................................................................................... 16

4.10.2 Repeatability (r) (95 % confidence) ............................................................... 16

4.10.3 Reproducibility (R) (95 % confidence) ............................................................ 16

---------------------- Page: 4 ----------------------
IEC 61125:2018 © IEC 2018 – 3 –

Annex A (normative) Thermometer specifications ................................................................ 20

Annex B (informative) Method for evaluating the oxidation stability of inhibited

insulating liquids in the delivery state by measurement of the induction period with

oxygen .................................................................................................................................. 21

B.1 Outline of the method ............................................................................................ 21

B.2 Reagents and test conditions ................................................................................ 21

B.3 Procedure ............................................................................................................. 21

B.3.1 General ......................................................................................................... 21

B.3.2 Preparation of the test ................................................................................... 21

B.3.3 Oxidation ....................................................................................................... 22

B.3.4 Determination of the induction period with oxygen ......................................... 22

B.3.5 Determinations on the oxidized oil (optional).................................................. 22

B.4 Report................................................................................................................... 23

B.5 Precision ............................................................................................................... 23

B.5.1 General ......................................................................................................... 23

B.5.2 Relative repeatability (r) (95 % confidence) ................................................... 23

B.5.3 Relative reproducibility (R) (95 % confidence) ............................................... 23

Annex C (informative) Method for evaluation of thermo-oxidative behaviour of unused

ester insulating liquids .......................................................................................................... 24

C.1 Outline of the method ............................................................................................ 24

C.2 Equipment ............................................................................................................ 24

C.2.1 Heating arrangement ..................................................................................... 24

C.2.2 Test vessels .................................................................................................. 24

C.2.3 Reagents ....................................................................................................... 24

C.3 Test procedure ...................................................................................................... 24

C.3.1 Sample conditioning and preparation ............................................................. 24

C.3.2 Ageing procedure .......................................................................................... 25

C.4 Determination of the oxidized insulating liquid ....................................................... 25

C.4.1 Soluble acidity ............................................................................................... 25

C.4.2 Dielectric dissipation factor (DDF) at 90 °C .................................................... 25

C.4.3 Appearance ................................................................................................... 25

C.4.4 Kinematic viscosity ........................................................................................ 25

C.5 Report................................................................................................................... 25

C.6 Precision ............................................................................................................... 26

Bibliography .......................................................................................................................... 27

Figure 1 – Typical 8 hole (4 x 2) aluminium heating block .................................................... 17

Figure 2 – Aluminium alloy temperature measuring block ...................................................... 17

Figure 3 – Position of the tube in the oil bath ........................................................................ 18

Figure 4 – Oxidation tube or absorption tube ........................................................................ 18

Figure 5 – Oxidation tube and absorption tube assembly ...................................................... 19

Figure C.1 – Headspace vial with copper catalyst ................................................................. 25

Table 1 – Repeatability and reproducibility of the oxidation stability test of uninhibited

mineral oil in the delivered state for 164 h at 120 °C ............................................................. 16

Table A.1 – Thermometer specifications ............................................................................... 20

Table B.1 – Precision data for induction time with oxygen for the oxidation test for

mineral oil according to Annex B ........................................................................................... 23

---------------------- Page: 5 ----------------------
– 4 – IEC 61125:2018 © IEC 2018

Table C.1 – Precision data for headspace procedure according to Annex C .......................... 26

---------------------- Page: 6 ----------------------
IEC 61125:2018 © IEC 2018 – 5 –
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
INSULATING LIQUIDS – TEST METHODS FOR OXIDATION STABILITY
Test method for evaluating the oxidation stability of insulating
liquids in the delivered state
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

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patent rights. IEC shall not be held responsible for identifying any or all such patent rights.

International Standard IEC 61125 has been prepared by IEC technical committee 10: Fluids

for electrotechnical applications.
This second edition cancels and replaces the first edition published in 1992 and
Amendment 1:2004. This edition constitutes a technical revision.

This edition includes the following significant technical changes with respect to the previous

edition:

a) the title has been modified to include insulating liquids different from mineral insulating

oils (hydrocarbon);
b) the method applies for insulating liquids in the delivered state;
c) former Method C is now the main normative method;

d) precision data of the main normative method has been updated concerning the dissipation

factor;
---------------------- Page: 7 ----------------------
– 6 – IEC 61125:2018 © IEC 2018
e) former Method A has been deleted;
f) former Method B has been transferred to Annex B;

g) a new method evaluating the thermo-oxidative behaviour of esters is included in Annex C.

The text of this standard is based on the following documents:
FDIS Report on voting
10/1047/FDIS 10/1052/RVD

Full information on the voting for the approval of this International Standard can be found in

the report on voting indicated in the above table.

This document has been drafted in accordance with the ISO/IEC Directives, Part 2.

The committee has decided that the contents of this document will remain unchanged until the

stability date indicated on the IEC website under "http://webstore.iec.ch" in the data related to

the specific document. At this date, the document will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.

IMPORTANT – The 'colour inside' logo on the cover page of this publication indicates

that it contains colours which are considered to be useful for the correct

understanding of its contents. Users should therefore print this document using a

colour printer.
---------------------- Page: 8 ----------------------
IEC 61125:2018 © IEC 2018 – 7 –
INSULATING LIQUIDS – TEST METHODS FOR OXIDATION STABILITY
Test method for evaluating the oxidation stability of insulating
liquids in the delivered state
1 Scope

This document describes a test method for evaluating the oxidation stability of insulating

liquids in the delivered state under accelerated conditions regardless of whether or not

antioxidant additives are present. The duration of the test can be different depending on the

insulating liquid type and is defined in the corresponding standards (e.g. in IEC 60296,

IEC 61099, IEC 62770). The method can be used for measuring the induction period, the test

being continued until the volatile acidity significantly exceeds 0,10 mg KOH/g in the case of

mineral oils. This value can be significantly higher in the case of ester liquids.

The insulating liquid sample is maintained at 120 °C in the presence of a solid copper catalyst

whilst bubbling air at a constant flow. The degree of oxidation stability is estimated by

measurement of volatile acidity, soluble acidity, sludge, dielectric dissipation factor, or from

the time to develop a given amount of volatile acidity (induction period with air).

In informative Annex B, a test method for evaluating the oxidation stability of inhibited mineral

insulating oils in the delivered state by measurement of the induction period with oxygen is

described. The method is only intended for quality control purposes. The results do not

necessarily provide information on the performance in service. The oil sample is maintained

at 120 °C in the presence of a solid copper catalyst whilst bubbling through a constant flow of

oxygen. The degree of oxidation stability is estimated by the time taken by the oil to develop a

determined amount of volatile acidity (induction period with oxygen). Additional criteria such

as soluble and volatile acidities, sludge and dielectric dissipation factor can also be

determined after a specified duration.

In informative Annex C, a test method intended to simulate the thermo-oxidative behaviour of

ester insulating liquids (headspace of air at 150 °C for 164 h) is described.

Additional test methods such as those described in IEC TR 62036 based on differential

scanning calorimetry can also be used as screening tests, but are out of the scope of this

document.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their

content constitutes requirements 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.

IEC 60247, Insulating liquids – Measurement of relative permittivity, dielectric dissipation

factor (tan δ) and d.c. resistivity

IEC 62021-2, Insulating liquids – Determination of acidity – Part 2: Colorimetric titration

IEC 62021-3, Insulating liquids – Determination of acidity – Part 3: Test methods for non-

mineral insulating oils
---------------------- Page: 9 ----------------------
– 8 – IEC 61125:2018 © IEC 2018

IEC 60422:2013, Mineral insulating oils in electrical equipment – Supervision and

maintenance guidance
ISO 383, Laboratory glassware – Interchangeable conical ground joints

ISO 4793, Laboratory sintered (fritted) filters – Porosity grading, classification and designation

ISO 6344-1, Coated abrasives – Grain size analysis – Part 1: Grain size distribution test

ISO 3104, Petroleum products – Transparent and opaque liquids – Determination of kinematic

viscosity and calculation of dynamic viscosity
ASTM E287, Standard specification for laboratory glass graduated burets
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following

addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
3.1
unused insulating liquid

insulating liquid that has not been used in, or been in contact with electrical equipment or

other equipment not required for manufacture, storage or transport
Note 1 to entry: See also IEC 60296, IEC 61099 and IEC 62770.
3.2
recycled insulating liquid

insulating liquid previously used in electrical equipment that has been subjected to re-refining

or reclaiming (regeneration) off-site

Note 1 to entry: Any blend of unused and recycled oils is to be considered as recycled.

3.3
oxidation stability

ability of an insulating liquid to withstand oxidation under thermal stress and in the presence

of oxygen and a copper catalyst

Note 1 to entry: Oxidation stability gives general information about the stability of the insulating liquid under

service conditions in electrical equipment. The property is defined as resistance to formation of acidic compounds,

sludge and compounds influencing the dielectric dissipation factor (DDF) under given conditions. Test durations for

insulating liquids are described in the corresponding standards.
3.4
induction period with air

graphical representation of the oxidation rate over the entire period which can be obtained by

titrating volatile acidity daily (or at other suitable time interval) and plotting the cumulated

results against time

Note 1 to entry: The induction period with air is determined by reading the time corresponding to 0,10 mg KOH/g

volatile acidity in the case of mineral oil. In the case of ester liquids a higher value needs to be established.

---------------------- Page: 10 ----------------------
IEC 61125:2018 © IEC 2018 – 9 –
3.5
volatile acidity

measurement of the amount of oxidation products collected in the water phase in the

absorption tube
3.6
soluble acidity

acidity (neutralization value) of oil as a measure of the acidic degradation products in the

insulating liquid

Note 1 to entry: The acidity of an oxidized oil is due to the formation of acidic oxidation products. Acids and other

oxidation products will, in conjunction with water and solid contaminants, affect the

...

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