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THE 8 t h INTERNATIO N AL SYMPOSIUM ON A DVANCED TOPICS IN ELEC T

THE 8 th INTERNATION AL SYMPOSIUM ON ADVANCED TOPICS IN ELEC TRICAL ENGINEERING May 23-25, 2013 Bucharest, Romania

Thermal Ageing

Effects on the Dielectr ic Properties

and Moisture Co ntent of Vegetable and Mineral Oil Used In Power Transformer s

Laurentiu Marius Dumitran 1 , M ember IEEE, Alexandra Ciuriuc 1 and Petru V. Noting her 1 , Member IEEE 1 University POLI TEHNICA of Bucharest, Laboratory of Electrical Mat erial, Splaiul In dependentei, No. 313, 060042, Bucharest, Romania dumitran@elma t.pub.ro, aciuriuc@elmat.pub.ro, petrunot@elmat.pub .ro

Abstract- The operational safety of transmiss ion and distribution

grids depends essentially on the power t ransformers’ state. Lately, there is a tendency to replace minera l oils with vegetable oils because vegetable oils provide a high er explosion safety

aspect for transformers due to their higher

vegetable oils are favorable for the enviro nment due to their

higher biodegradability. The focus of the

study the properties of mineral and vegetabl e after these oils are exposed to accelerated thermal ageing. Veg etable and mineral oil samples were subjected to accelerated th ermal ageing (with and without cellulosic paper) at three diffe rent temperatures:

present paper is to

fire points. Further,

135 °C, 155 °C and 175 °C. The dielectri c properties of the samples (relative permittivity, loss factor a nd resistivity) and their water content were determined fo r different ageing durations. The results show that in the c ase of mineral oil

the water content

samples, there is a direct relation between

values and the dielectric properties. How ever, the obtained results indicate that the water content does n ot fully characterize the ageing condition of vegetable oil.

Keywords: power transformers, vegetable

oils,

thermal ageing, dielectric properties, water c ontent

and

mineral

I.

INTRODUCTION

In recent years, the use of vegetable oils instead of mineral

a majority of the transmission and

distribution grids have mineral oil i mpregnated paper insulation and a large volume of miner al oil is used [1].

Although mineral oil has excellent electri c properties and a good thermal stability that has been p roven over time, environmental considerations in recent t imes have always

[2]. Conventional refining and they

are usually non-biodegradable and can har m the environment for many years.

(or natural esters)

raised a concern on their continuous usage mineral oil is obtained through petroleum

oil is gaining a lot of attention. Today, power transformers which operate in

From this point of view, vegetable oils

appear to meet the requirements necess ary for insulation systems of power transformers. First of all, vegetable oils that are specially designed for electric insulatio n and heat transfer purpose, have high biodegradability the reby causing less harm to the environment. In addition, the y increase the fire- safety aspect in transformers due to thei r higher fire-point values as compared to mineral oil and the y have appropriate electric properties and thermal stability [2 -4]. However, the continuous use of vegetable oils in ins ulation systems of

978-1-4673-5980-1/13/$31.00 ©2013 IEEE

a good knowledge of their

behavior over time. Perform ance of vegetable oils in

combination with cellulosic pa per and stability of these oils under thermal, electric and en vironmental stress should be understood. Information concerning the g eneral properties of vegetable

oint etc.) is presented in [5-7], oils is analyzed in [2]. In a

previous study [8], it has b een shown that the electric properties of vegetable oil (th e relative permittivity ε r ’ and loss factor tgδ) under accelerat ed thermal stress increase with

ageing time and temperature.

effect on the electric properties of vegetable oils and mixtures

of mineral and vegetable oils ha ve been discussed in literature

[4-7, 9-15]. Numerous studies

water content, permittivity, los s factor, electric conductivity and breakdown voltage with res pect to the ageing temperature

and duration have also been Generation of acids in natural

also been discussed [5, 7, 16]. Acids are known to be one of the ageing by-products of ce llulosic paper and oils. The autocatalytic effect of the acids accelerates the ageing process

of the oil and paper which

can influence the measured

properties [16, 17]. It has been shown that paper in vegetable

low molecular weight acids

oil contains fewer amounts of

compared to the case with min eral and this is an advantage for vegetable oils because thes e acids are very dangerous for cellulose-based products [5]. Li fetime estimation of vegetable oil is presented in [2] and sever al comparative studies focused on the properties of mineral, sil icone and vegetable oils [4, 6, 11-12, 15, 18].

on the effect of accelerated

concerning the variations of

oils (viscosity, flash and fire p and the gas content of these

power transformers requires

The moisture content and its

reported [4, 6-7, 12, 14-15]. esters under thermal stress has

The present paper focuses

thermal stress on the electric pr operties (real part of complex permittivity, loss factor and res istivity) and moisture content of vegetable oil. Possible corr elations between the variation of electric properties and mois ture content are investigated. Samples of vegetable oil w ere subjected to accelerated

thermal ageing and the electric

properties and water content

were determined at different a geing durations. For a better

understanding, the obtained r esults for vegetable oil were compared with those of miner al oil samples aged under the same conditions.

Fig. Fig. 1. 1. The The hydrolysis hydrolysis reaction reaction of of vegetable vegetable oils

Fig. Fig. 1. 1. The The hydrolysis hydrolysis reaction reaction of of vegetable vegetable oils oils [20] [20]

II. AGEING MECHANISMS OF OILS

When power transformers are in operation, their insulation systems consisting of oil and paper are subjected to different stresses. Amongst these stresses, thermal stress is the most important because it causes degradation reactions, thereby worsening the properties of the oil. Vegetable oils used for electric insulation are based on triglyceride chemistry with saturated and unsaturated fatty acids attached to the glycerol backbone [8]. Due to the nature of the chemical structure, vegetable oils are more hygroscopic and can also undergo hydrolysis. Further, vegetable oils are also prone to oxidation wherein, the rate of oxidation depends on the types and concentration of fatty acids. The main reactions that cause the degradation of the vegetable oil are oxidation and hydrolysis, and the resulting by-products are gases (CO, CO 2 ), water and acids [19]. The unsaturated bonds in the fatty acids lower the oxidation stability of the natural ester because the oxygen molecule disrupts the fatty acid at the carbon double bond. Therefore, for higher un-saturation levels, the number of double bonds is higher and the oil becomes more susceptible to oxidation [20]. Besides oil ageing, the degradation of the cellulose paper should also be taken into account because the resulting by- products reach the oil and change its properties. Due to the influence of temperature, chemical reactions take place in cellulosic paper, and several by-products like CO, CO 2 , H 2 O, H 2 , CH 4 and furans are generated [8]. Water, which is a by-product of oil and paper degradation reactions, can exist in transformers in different states. Most of the water in oil is found in the dissolved state. After it exceeds the saturation value, free water precipitated from the oil will be found in suspension or drops [21]. The moisture content in the oil can be characterized by the absolute (w abs ) and, relative (w rel ) values. The relative moisture content in oil is represented by the ratio of the absolute moisture content (w abs ) of oil for a given temperature T and the saturation water content at the same temperature T (w L (T)) [14]:

content at the same temperature T ( w L ( T )) [14]: Fig. 2. Trans-esterification

Fig. 2. Trans-esterification of cellulose [20].

C n H 2n+2 C n H 2n + H 2

Alkane Alkene + Hydrogen

C m+n H 2(m+n)+2 C m H 2m + C n H 2n+2.

n-Alkane

Alkene + Alkane

Fig. 3. Cracking and dehydrogenation reactions of mineral oil.

w

rel

=

w abs

w (T)

L

.

(1)

At room temperature, the saturation limit of vegetable oil is about 3000 mg/kg, compared to 60 mg/kg for mineral oil [20]. Due to this significant difference, even though the vegetable oil has absolute moisture content higher than mineral oil, the relative moisture content of the vegetable oil is much lower. This could have a positive effect on the global insulation system because the vegetable oil absorbs the water from the paper and in this way it keeps the paper drier. Moreover, the hydrolysis reaction (Fig. 1) that takes place in the oil is also beneficial for the cellulose insulation. The free fatty acids that are formed in the vegetable oil as a result of the hydrolysis reaction participate in a trans-esterification reaction in the cellulose (Fig. 2). The reactive hydroxyl groups on the cellulose molecule become esterified with fatty acids in vegetable oil and it prevents the paper from further degradation [20]. Concerning the degradation of the mineral oil, this topic was much studied and is better known. The main reactions that lead to the degradation of the mineral oil are the cracking reaction (which leads to the C-C bonding scission and forms alkanes and alkenes), oxidation and dehydrogenation (Fig. 3) [8]. High temperature accelerates the mineral oil oxidation and some metals like copper act as a catalyst. The presence of oxygen can degrade the hydrocarbons through processes based on free radical reactions, which generate hydro peroxides [22, 23] which are unstable and decompose to free radicals finally leading to the appearance of water, ketones and other by-products [24].

III. EXPERIMENTAL SET-UPS AND SAMPLES

The experiments were performed on commercially available natural ester and mineral oil meant for power transformer applications. In order to perform the ageing of the oil samples, 15 controlled clean stainless steel ageing cells were used. The first five of these were filled with vegetable oil, the next five cells were filled with vegetable oil and 10 samples of 0.25 mm thick Weidmann cellulose paper and the last five cells were filled with mineral oil. Each ageing cell contained 8.4 grams of paper, 9 grams of copper and 23 grams of iron. Further, for clarity, the investigated oil samples will be called A – vegetable oil aged in presence of copper and iron, B – vegetable oil aged in presence of cellulosic paper, copper and iron and C – mineral oil aged in presence of copper and iron.

10.0 9.5 9.0 8.5 8.0 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0
10.0
9.5
9.0
8.5
8.0
7.5
7.0
6.5
6.0
5.5
5.0
4.5
4.0
3.5
3.0
2.5
2.0
0 200
400
600
800 1000 1200 1400 1600
Real part of relative permittivty

Ageing time (h)

Fig. 4. Variation of real part of relative permittivity for A samples ( , , ), and B samples ( , , ) aged at 135 °C ( , ), 155 °C ( , ) and 175 °C ( , ) for f = 1 mHz.

All ageing cells, fully sealed, were introduced in the drying oven at three different temperatures (135 °C, 155 °C and 175 °C) for a total of 1250 h. Three ageing cells containing each type of sample (A, B and C) were extracted every 250 h and the following properties of the oils were determined: the real part of the complex relative permittivity ε r ’, the loss factor tgδ, the resistivity ρ and the absolute water content w abs . The resistivity of the oil’s samples was calculated using the values of absorption/resorption currents [8] measured with a Keithley 6517 electrometer and an Irlab liquid measuring cell. The value of the DC applied voltage was U 0 = 40 V. In order to determine the dielectric loss factor and the components of the complex relative permittivity, a Novocontrol impedance analyzer was used. The applied voltage had the value of 1V and the electric field frequency was in the range of 10 -3 – 10 3 Hz. The ambient temperature during the measurements was 28°C. The absolute water content was measured using a Karl-Fischer coulometer.

450 400 350 300 250 200 150 100 50 0 0 200 400 600 800
450
400
350
300
250
200
150
100
50
0
0 200
400
600
800 1000 1200 1400 1600
Loss factor

Ageing time (h)

Fig. 5. Variation of the loss factor for A samples ( , , ), and B samples ( , , ) aged at 135 °C ( , ), 155 °C ( , ) and 175 °C ( , ) for f = 1 mHz.

1.6 1.4 1.2 1 0.8 0.6 0.4 0.2 0 0 200 400 600 800 1000
1.6
1.4
1.2
1
0.8
0.6
0.4
0.2
0
0
200
400
600
800
1000 1200 1400 1600
Resistivity · 10 -11 (ohm·m)

Ageing time (h)

Fig. 6. Variation of resistivity for A samples ( , , ), and B samples ( , , ) aged at 135 °C ( , ), 155 °C ( , ) and 175 °C ( , ) (U 0 = 40 V).

IV. RESULTS AND DISCUSSIONS

Figs. 4-6 present the variations of electric properties of samples A and B of vegetable oil as a function of ageing duration, τ. It can be seen that the values of ε r ’ and tgδ quantities increase with ageing time. Also, the increase in ε r ’ and tgδ with ageing time is more pronounced at higher temperatures. On the other hand, the resistivity decreases with time and this variation is faster at higher temperatures. Obviously, for A samples, these changes in the electric properties are exclusively due to the vegetable oil degradation which has no contact with the environment during ageing process. In the case of B samples, the degradation by- products of cellulosic paper which reach the oil can also modify the measured properties. The increase of the real part of complex relative permittivity (Fig. 4) may have a common reason based on the increase in polar by-products of chemical degradation reactions. For lower temperature (135 o C and 155 o C) and ageing duration shorter than 1000 h, the variation of ε r ’ is not significant which means that no important degradation rate exists. However, for 175 o C, ε r ’ strongly increases and that indicates an accelerated degradation process. Fig. 5 indicates that the vegetable oil’s loss factor increases steeply with ageing time. This shows that polarization and conduction phenomena intensify in time (especially for samples submitted to 175 o C). Fig. 6 shows the decrease of the oil’s resistivity with the ageing time which is due to the increase of charge carrier’s concentration as a result of degradation process. In the case of the tgδ and ρ properties, there are three obvious distinct intervals (dependent on the ageing temperature) in which the values of the properties for samples B are higher or lower than those of samples A (Table 1). In the first interval (I), the loss factor and resistivity values for vegetable oil aged in the presence of paper (respectively, tgδ B

5.0 4.8 4.6 4.4 4.2 135 °C 4.0 3.8 155 °C 3.6 3.4 175 °C
5.0
4.8
4.6
4.4
4.2
135 °C
4.0
3.8
155 °C
3.6
3.4
175 °C
3.2
3.0
2.8
0 200
400
600
800
1000 1200 1400 1600
Real part of relative permittivity

Ageing time (h)

Fig. 7. Variation of the real part of complex relative permittivity of C samples aged at 135 o C ( ), 155 o C ( ) and 175 o C ( ) as a function of ageing time (f = 1 mHz).

and ρ B ) are higher than those corresponding to the samples aged in the absence of paper (tgδ A and ρ A ). This could be due to the absorption of water in paper and to the increase of the concentration and mobility of electric dipoles and charge carriers.

TABLE I

LOSS FACTOR AND RESISTIVITY FOR A AND B OIL SAMPLES FOR DIFFERENT AGEING TIME τ

Ageing time [h]

 

I

 

II

III

T

= 135 o C

0

- 500

500

- 1200

> 1200

T

= 155 o C

0

- 350

350

- 600

> 600

T

= 175 o C

0

- 300

300

- 500

> 500

tgδ B : tgδ A

tgδ B > tgδ A

tgδ B < tgδ A

tgδ B > tgδ A

 

ρ B : ρ A

ρ B > ρ A

ρ B < ρ A

ρ B > ρ A

At higher ageing durations (interval II), part of the water is consumed in the hydrolysis reaction, which leads to an increase of tgδ and ρ values for samples A compared to samples B. During interval III, the paper degradation contributes more to the increase of charge carrier’s

140 120 100 155 °C 80 60 175 °C 40 20 135 °C 0 0
140
120
100
155 °C
80
60
175 °C
40
20
135 °C
0
0 200
400
600
800
1000 1200 1400 1600
Loss factor

Ageing time (h)

Fig. 8. Variation of the loss factor of C samples aged at 135 o C ( ), 155 o C ( ) and 175 o C ( ) as a function of ageing time (f = 1 mHz).

5.0 4.5 4.0 175 °C 3.5 155 °C 3.0 135 °C 2.5 2.0 1.5 1.0
5.0
4.5
4.0
175 °C
3.5
155 °C
3.0
135 °C
2.5
2.0
1.5
1.0
0.5
0.0
0 200
400
600
800
1000
1200
1400
1600
Resistivity·10 -11 (ohm·m)

Ageing time (h)

Fig. 9. Variation of the resistivity for C samples aged at 135 o C ( ), 155 o C ( ) and 175 o C ( ) as a function of ageing time (U 0 = 40 V).

concentration, which determines an increase of tgδ and ρ values for the B samples compared to the A samples. This model is verified completely in the case of the tests performed at 175 o C and partially for the ones performed at 155 o C and 135 o C. The variations of electric properties of mineral oil samples aged under same conditions were investigated and are presented in Figs. 7 -9. As expected, the quantities ε r ’ and tgδ increase with τ while the resistivity decreases. Similar results were presented in [25] and indicate that a degradation process

takes place in mineral oil submitted to thermal stress. Given that the ageing of mineral oil was done in sealed cells, (like in

the case of A and B samples), the variations of mineral oil’s electric properties are exclusively due to the by-products which result from chemical degradation reaction of the oil. Figures 10-12 present the variation of absolute moisture content as a function of ageing time in samples A, B and C respectively. As it can be seen in Fig. 10, in the case of the vegetable oil aged at 135 °C and 155 °C, the water content increases in the first 300 hours of ageing and then decreases for the rest of the ageing time. Similar results were presented in [15]. This variation can be explained by the different

330 300 270 240 210 135 °C 180 150 120 155 °C 90 175 °C
330
300
270
240
210
135 °C
180
150
120
155 °C
90
175 °C
60
30
200
400
600
800
1000 1200 1400 1600
Water content (ppm)

Ageing time (h)

Fig. 10. Variation of water content of A samples aged at 135 o C ( ), 155 o C ( ) and 175 o C ( ) as a function of ageing time.

200 180 160 155 °C 140 120 100 175 °C 80 60 135 °C 40
200
180
160
155 °C
140
120
100
175 °C
80
60
135 °C
40
20
0 200
400
600
800
1000 1200 1400 1600
Water content (ppm)

Ageing time (h)

Fig. 11. Variation of water content of B samples aged at 135 o C ( ), 155 o C ( ) and 175 o C ( ) as a function of ageing time.

degradation reactions that take place in the vegetable oil: at the beginning of the ageing process the water content increases due to the degradation process and after this period, the hydrolysis reaction takes place and it consumes the water from the oil [15]. This reaction leads to the formation of free fatty acids. Therefore it can be assumed that during the whole ageing process the acidity of the oil increases [15], which, taking into account that the free fatty acids are polar compounds, could have an influence on the value of the permittivity. In the case of the samples aged at 175 °C, the absolute water content is very low, and that can be probably given by the fact that the hydrolysis reaction is more intense at a higher temperature. As it can be seen in Fig. 11, the water content of oil aged in presence of cellulosic paper takes lower values compared to those obtained for A samples. This difference can be explained by the fact that the vegetable oil was aged in the presence of paper and the trans-esterification reaction of the cellulose has to be taken into account. During the first 200 – 300 hours of ageing the water content increases rapidly due

40 35 30 25 135 °C 20 175 °C 155 °C 15 10 0 200
40
35
30
25
135 °C
20
175 °C
155 °C
15
10
0 200
400
600
800 1000 1200 1400 1600
Water content (ppm)

Ageing time (h)

Fig. 12. Variation of water content of C samples aged at 135 o C ( ), 155 o C ( ) and 175 o C ( ) as a function of ageing time

60 50 40 C 30 20 A B 10 0 0 200 400 600 800
60
50
40
C
30
20
A
B
10
0
0 200
400
600
800 1000 1200 1400 1600 1800
Relative water content (%)

Ageing time (h)

Fig. 13. Variation of relative water content of A ( ), B ( ) and C ( ) samples as a function of ageing time.

to the transfer of the water from the paper to oil (because of the high temperature value). For the following 500 – 700 hours of ageing, the water content decreases due to the hydrolysis reaction and for the rest of the ageing process it increases again because more water resulted from the trans- esterification reaction of cellulose is transferred in oil [20]. Regarding the water content in the mineral oil samples (Fig. 12), it can be seen that for the temperatures of 135°C and 155 °C, w abs increases with the ageing time. In the case of T = 175 °C, it can be seen a pronounced increase of the water content during the first 200 hours of ageing, followed by a decrease to around 21 ppm. During the last part of the ageing process (after 650 hours) the water content starts increasing again and this is most probably due to the oil degradation

[18].

Examining Figs. 7 and 12, it results that in the case of mineral oil, it can be distinguished a correlation between the water content in oil and its real part of relative permittivity and loss factor variations. Thereby, during the first time interval (τ 1 , depending of the ageing temperature) the water content and ε r ’ increase, in the following time interval τ 2 they decrease, and in the last part of ageing (τ > τ 2 ) they increase again. Based on this observation it results that the increases of ε r ’ and tgδ in the last period of ageing time, are given, among others factors, by the water which is present in the oil. Fig. 13 presents the variation of relative water content w rel as a function of ageing time for mineral oil and vegetable oil aged without and with paper (samples A and B) at T = 135 °C. It results that w rel is significantly lower in the case of vegetable oil compared to the values obtained for mineral oil. Also, it can be seen that, while the relative water content for mineral oil increases in time, in the case of vegetable oil, w rel increases during the first 350 h and then slowly decreases for the rest of the ageing time. Looking at these results, it appears that while in the case of mineral oil, a direct correlation is observed between the relative water content and electric

properties, but, in the case of vegetable oil such a link is not evident. Based on these results, it appears that the estimation of vegetable oil ageing condition based on the relative or absolute water content seems to be erroneous.

V.

CONCLUSIONS

The results presented in this paper confirm that thermal ageing results in a variation in the electric properties and moisture content of vegetable and mineral oils. Also, a correlation between the variation of absolute and relative moisture content of mineral oil is observed on one side, and the variation of its electric properties, on the other side. In the case of vegetable oil, it has been observed that there is no evident relationship between the absolute and relative water content with the dielectric properties. It means that the water content is not an appropriate diagnostic factor to estimate the ageing condition of vegetable oil. A possible explanation could be that the water content does not contribute to a variation in the dielectric properties of the oil, but the variation is due to the degradation products resulting from the chemical reactions that take place between water and oil (with or without paper).

ACKNOWLEDGMENT

This work has been supported by the Sectorial Operational Programme Human Resources Development 2007-2013 of the Romanian Ministry of Labour, Family and Social Protection through the Financial Agreement POSDRU/89/1.5/S/62557, POSDRU/107/1.5/S/76903.

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