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Corrosive Sulphur IEC

The document discusses technical specifications and test methods for insulating oils according to IEC 60296 standards. It provides details on revisions made between editions 2 and 3 of the standard, including new test methods for properties like viscosity, pour point, and oxidation stability. Various test procedures are described, such as those for acidity, corrosion of copper, and oxidation stability testing. Performance results are shown for insulating oils used in Austrian transformers. The document also discusses phenomena like copper corrosion in transformers and mineral oil chemistry.
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0% found this document useful (1 vote)
425 views61 pages

Corrosive Sulphur IEC

The document discusses technical specifications and test methods for insulating oils according to IEC 60296 standards. It provides details on revisions made between editions 2 and 3 of the standard, including new test methods for properties like viscosity, pour point, and oxidation stability. Various test procedures are described, such as those for acidity, corrosion of copper, and oxidation stability testing. Performance results are shown for insulating oils used in Austrian transformers. The document also discusses phenomena like copper corrosion in transformers and mineral oil chemistry.
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Technical Market Support

The NOVA Grades


Presentation
Dipl.Ing.Gerfrid Newesely Gmunden, 27.Feb.2007

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IEC 60296 Ed.2/1982


Properties Kinematic viscosity, mm 2/s at 40 C at -15 C at -30 C at -40 C Limits Class IA Class IIA Class IIIA < 16,5 < 11,0 < 3,5 --< 800 -< 1.800 ---< 150 > 140 > 130 > 95 < -30 < -45 < -60 clear, free from sediment and suspend matter < 0,895 > 40; see note < 0,895 Non - corrosive 30 / 40; see note 0; 0,3; see note see note > 30 > 50 < 0,005

Flash point, C Pour point, C Appearance Density, kg/dm 3 at 20 C Interfacial tension, N/m at 25 C Neutralisation number, mg KOH/g Corrosive sulphur Water content, mg/kg Anti-oxidant additives Oxidation stability Breakdown voltage: as delivered, kV after treatment, kV Dissipation factor, at 90 C and 40 to 60 Hz
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Revision Requirements

Viscosity classification, Pour point etc. Acidity test Corrosive sulfur test Oxidation stability criterions New requirements

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IEC 60296 Ed.3/2003


Properties Transformer Oil Kinematic viscosity, (LCSET) C mm /s at 40 at -30 C at -40 C Pour point, C Water content, mg/kg Breakdown voltage, kV Dissipation factor, at 90 C and 40 to 60 Hz Appearance Acidity, mg KOH/g Interfacial tension, mN/m at 25 C Total sulphur Corrosive sulphur Anti-oxidant additives, % 2-Furfural content, mg/kg Oxidation stability Total acidity, mg KOH/g Sludge, % DDF / 90 C Test duration, h Gassing Flash point, C Density, g/ml at 20 C PCA PCB
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Limits Low Temp. Switchgear Oil

max. 3,5 -max. 400 max. -60 max. 30 / max. 40 min. 30 / min. 70 max. 0,005 clear, free from sediment and suspend matter max. 0,01 min. 40; see note No general requirement Non corrosive 0 (U) / 0 - 0,08 (T) / 0,08 - 0,4 (I) ; see note max. 0,1 max. 1,2 max. 0,8 max. 0,500 164 (U) / 332 (T) / 500 (I) ; see note No general requirement min. 135 min. 100 max. 0,895 max. 3% DMSO Extract Not detectable

max. 12 max. 1.800 -max. -40

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IEC 60296 Ed.3/2003


Lowest cold start energizing temperature (LCSET)

LCSET 0 C -20 C -30 C -40 C

Max. viscosity 1800 mm 2/s 1800 mm 2/s 1800 mm 2/s 2500 mm 2/s

Max. pour point -10 C -30 C -40 C -50 C

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Neutralisation number
Coulometric titration (IEC 296 Ed.2/1982)

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IEC 62021-1 Acidity


Potentiometric method

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IEC 62021-1 Acidity


Potentiometric method

Touch control screen or PC monitor control available


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Corrosive Sulphur ASTM D 1275

250 ml Oil Cu Strip 140 C 19 hrs

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Corrosive sulphur Test ISO/ASTM

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Corrosive sulphur
Copper strip / Silver strip

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Corrosive sulphur
DIN 51353

100 ml Oil Ag strip 100 C 18 h

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IEC 60296 Ed.2 Oxidation tests


Test Conditions Measured Criterions

IEC 61125 A 100 C (IEC 74) 30 cm Cu 1 l O2 /h IEC 61125 B 120 C (IEC 474) 90 cm Cu 1 l O2 /h
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Acidity Sludge

Induction period (until volatile acids have neutralized the caustic solution)

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IEC 60296 Ed.2 Oxidation tests


IEC 61125A (uninhibited oils) Test duration: 164 hours
Oxygen, 1l/min

Test temperature: 100 C


25 ml oil

Limits:
30 cm Cu-wire Acidity: max. 0,4 ml KOH/g oil Sludge: max. 0,1 %
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IEC 60296 Ed.2 Oxidation tests


IEC 61125B (inhibited oils) Test duration: see Induction period
Oxygen, 1l/min

Test temperature: 120 C

Caustic solution (corresponding to 0,28 mg KOH/g oil) 25 ml oil + indicator

90 cm Cu-wire

Limit:
Induction period: min 120 hrs until change of colour

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IEC 60296 Ed.3 Oxidation tests

Test

Condition

Measured Criterions

IEC 61125 C 120 C (IEC 813) 90 cm Cu 0,15 l Air /h

Total acidity (soluble+volatile) Sludge Diel.Dissipation Factor

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IEC 60296 Ed.2 Oxidation tests


IEC 61125C (uninhibited and inhibited oils) Test duration: uninhibited: 164 hrs, inhibited 500 hrs
Air 0,15 l/min

Test temperature: 120 C


Distilled water 90 cm Cu-wire 25 ml oil soluble acid sludge DDF Volatile acid

Limits:
Total acids: max. 1,2 mgKOH/g Sludge: max. 0,8 % DDF: max. 0,500

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Limits:
2 options General specification
(for general application)

Specific Requirements
(for special application)

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IEC 60296 Ed.3/2003


Compilation of limits
General requirements Specific requirements Oxidation stability (IEC 1125 C) standard ox. stability high ox. stability max. 1,2 mg KOH / g max. 0,3 mg KOH / g max. 0,8 % max. 0,05 % max. 0,500 max. 0,050 --max. 0,15 % Electrostatic tendency ECT Gassing (IEC 60628 A) -------

total acidity sludge DDF / 90 C total sulphur to be agreed

uninhibited oils (U) trace inhib. oils (T) inhibited oils (I)
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Acidity of Nynas-Technol Insulating Oil


in service in transformers in the Austrian High Voltage Grid
0,18

0,16

0,14

0,12 NZ [mgKOH/g]

0,1

0,08

0,06

0,04

0,02

0 0 5 10 BLW 12 15 BLW 13 20 BLW 14 25 Jahre BLW 23 BLW 28 30 BLW 30 35 BLW 35 40 BLW 45 45 50

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Interfacial Tension of Nynas-Technol Insulating Oil


in service in transformers in the Austrian High Voltage Grid
45 40 35 30 25 20 15 10 5 0 0 5 10 15 20 25 Jahre BWL 12 BWL 13 BWL 14 BWL 23 BWL 28 BWL 30 BWL 35 BWL 48 30 35 40 45 50

Grenzflchenspannung [mN/m]

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Diel.Dissipation Factor of Nynas-Technol Insulating Oil


in service in transformers in the Austrian High Voltage Grid
45

40

35

30

tg delta

25

20

15

10

0 0 5 10 15 20 25 Jahre BLW 12 BLW 13 BLW 14 BLW 23 BLW 28 BLW 30 BLW 35 BLW 45 30 35 40 45 50

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The Copper Corrosion Phenomenon

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The Copper Corrosion Phenomenon:


Damages in Brazil

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The Copper Corrosion Phenomenon:


Damages in Brazil

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The Copper Corrosion Phenomenon:


Damages in Brazil

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The Copper Corrosion Phenomenon:


Damages in Brazil

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The Copper Corrosion Phenomenon:


Damages in Brazil

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The Copper Corrosion Phenomenon:


Criteria and indications

Strong indications:
Sealed or nitrogen blanketed transformers/reactors (rubber diaphragm equipped conservator, lack of oxygen) High operating ambient temperature but within design limits Transients In combination with certain components in oil

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The Copper Corrosion Phenomenon:


Criteria and indications Conditions where this phenomen is less likely to occur:

In open breathing transformers (conservators) When varnished copper is used The lower the temperature, the lower the risk

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Oil reactions
with copper
Low presence of oxygen and high temperatures will promote sulfur/copper reactions on the conductor surface and form deposits which might migrate to the inner cellulose layers. Oil soluble copper ions might migrate into the oil and form copper sulfide on the outside of the cellulose and/or spacers.

Copper ions dissolved in the oil Copper sulphide deposits on paper

+Sulfur Cu-Sulfide

Cu-ion

Paper

Reaction on copper surface can deposit on paper and penetrate to next layer
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Cu-Sulfide Copper

Development of Copper corrosion test methods: ABB - CCCD Test (Covered copper conductor deposition)

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Development of Copper corrosion test methods: ABB - CCCD Test (Covered copper conductor deposition)

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Development of Copper corrosion test methods: ABB - CCCD Test (Covered copper conductor deposition)
Results 1

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Development of Copper corrosion test methods: ABB - CCCD Test (Covered copper conductor deposition)
Results 2

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Mineral oil chemistry


Basic hydrocarbon structures in mineral oil

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Mineral oil chemistry

Theoretical molecules in naphthenic oil

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Sulphur containing molecules


Small sulphur containing molecules are more reactive than larger Small sulphur containing molecules are not present in transformer oils However, larger sulphur containing molecules are present in oils and are potentially reactive towards copper and some are acting as inhibitors R-SH R-S-R R-S-S-R

R R S
Decreased reactivity

R S

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Nitrogen containing molecules


Nitrogen are present in oil in various molecular structures Nitrogen molecules are potential promoters for copper migration and/or could act as copper passivators

R N N N

N
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Mineral Oil Chemistry


Hetero atoms in mineral oil molecules are necessary to achieve good oxidation stability

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Hydrotreatment Refining
- Optimization of properties

Need of optimization but you can not get everything


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A Modern Hydrotreatment Refinery

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Hydrotreating processes

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Tests of the new oil filled in one failed reactor

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Nynas Selected Passivator


Oil soluble BTA derivative Commercially available Developed for use in high temperature lube oil applications, e.g. turbine oil Protects copper and yellow metals

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Passivators: Test results


(ASTM 1275 B)

E = New Oil

A = New Oil

C = used Oil

H = Oil E passivated
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B = Oil A passivated after 15 h ageing

D = Oil C passivated

Technical solutions
In-service solutions Add passivator to transformers at risk: Halts any further degradation

Nynas TRO products Nynas offer special passivated products: Nytro 10GBN passivated Nytro 10 GBA passivated Nytro 10 GBX passivated

Nytro 10 XN Nytro 4000A/X


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Corrosivity Tests

Corrosive sulphur DIN*) Corrosive sulphur ASTM**) These methods are mainly developed to detect contaminants from manufacturing/handling of transformer oil. *)IEC 60296

DIN 51353 ASTM D1275

Potentially corrosive sulfur compounds in transformer oil ??

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Development of Copper corrosion test methods:


Copper strip method to detect corrosive and potentially corrosive sulphur in insulating oil

Corrosive sulphur ASTM D 1275

ASTM 1275 A 140 C 19 h

ASTM 1275 B 150 C 48 / 72 h

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Development of Copper corrosion test methods: CIGRE - CCD Test


for detection of potentially corrosive sulfur in insulating oil

Head space vial 15 ml Oil 30 mm Cu 150 C 72 h

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Development of Copper corrosion test methods: CIGRE - CCD Test


for detection of potentially corrosive sulfur in insulating oil

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NYNAS Product development strategy: Develop oils that meet all tests for corrosive and potentially corrosive sulphur in oil without passivator:

The NOVA Grades

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Hydrotreatment Refining
- Optimization of properties

Need of optimization but you can not get everything


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NYNAS - NOVA GRADES:


UNINHIBITED INHIBITED

SUPER

4000X Lyra X 10XN Gemini X Taurus Libra

HIGH

STANDARD

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NYNAS - NOVA GRADES:

UNINHIBITED

INHIBITED

Non Gasoil

Taurus

4000X Lyra X

Gasoil Gasoil Arctic Grade


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Libra

Gemini X 10XN

Technical Market Support

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