On-Line Reclamation of Aged

Transformer Oils
J. Sabau
INSOIL Canada, Ltd.

Abstract
The reclamation of aged transformer oils by Fullers Earth has long been practised by the electrical power industry. Although the major analytical properties of processed oil such as the dissipation factor at lOOOC, the interfacial tension (IFT) and the total acid number (TAN) improve to the level of new oils, the quality of reclaimed oil is considered to be doubtful. Consequently, conditionbased maintenance planners believe that purified liquid insulation can never regain the performance of new oil. This mistrust is fuelled by the fact that the existing testing procedures are not capable of establishing a quantitative relationship between oxidation stability and gassing tendency under electrical stress determined in laboratory conditions and the performance of oil in real life. Over the past years, the co-operation between certain state of the art instrument manufacturers and enhanced testing procedure developers has provided the electrical power industry with the means of eliminating this deficiency. This paper intends to show that the quality of properly reclaimed aged oils can successfully compete with that of new oils. Thus, in addition to extending the life cycle of a non-renewable resource, the on-line reclamation of liquid insulation might also prevent the premature ageing of paper insulation. Key Words. Aged transformer oil, Reclamation technology, Dissolved decay products, Particle counting, Oxidation test, Gassing tendency.

inhibitors has proven to be only a partial solution because, rather than preventing the decay of oil, the process is only retarded. The endeavours of service providers to control the damage by reclaiming the aged oils are currently hampered by missing testing procedures capable of reliably determining its effectiveness. One example is ASTM Standard Test Method for Oxidation Stability of Mineral Insulating Oil, Designation D 2440-99 [2], which in Section 1, Scope, states, This method is applicable to new oil, both uninhibited and inhibited, but is not well defined for used or reclaimed oils. New achievements that improve the chemistry of mineral insulating oils can provide the electrical power industry with an excellent opportunity to maximize the service reliability of high, and most importantly, of very high voltage ageing power transformers.

2 Theoretical Background

There is no doubt that the service reliability of power transformers largely depends upon the condition of the oil. The gradual deterioration of purity due to its ageing process has an important impact upon the paper insulation. The extent of the damage to the windings becomes obvious when its dielectrical properties are measured and compared to the values of the same transformer when it was commissioned. Since the relationship between the ageing of oil and the deterioration of the internal insulation is very seldom monitored, the growing amount of decay products reflected in the slowly changing analytical properties of aged oils is not currently considered to be a threat to the operational safety of power transformers. As a result, there is no consensus regarding the level at which these characteristics should be categorized as being too bad. As a result, the selective removal of decay products by 1 Introduction reclamation cannot be economically justified. In contrast, According to a paper published ten years ago by a what maintenance planners believe to be alarming is the team of Australian researchers [l], a major problem dissolved gas content in oil [3]. A closer examination of encountered world-wide by both producers and large the mechanism responsible for the genesis of all decay industrial consumers ,of electrical energy is the ageing of products, as well as certain new findings offered by an transmission and distribution power transformers. Nearly applied research project should stimulate a fresh half of them are now over 25 years old and it is an consideration of this relationship between the purity of oil accepted view that replacement is not an economically and the service reliability of power transformers. viable option. Since the large majority of these expensive machines are free breathing, with the exception of many sealed units in the US, the primary cause of ageing is considered to be the oxidation of oil. The use of oxidation

0-7803-7180-1/$10.00 02001 IEEE

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2.1 The Genesis of Decay Products

So long as vulnerable hydrocarbon chains are not broken due to the energy supplied by electrical stress the chemical energy of dissolved oxygen or both the initial properties of insulating oils remain unchanged [4]. While the electrical stress is a given in both free breathing and sealed transformers, the attack of oxygen is limited to the first type only. Since the impact of electrical stress on the stability of oil is not clearly understood, a priority has been given to the protection of liquid insulation against oxidation.

2.1.2 The Impact of Dissolved Oxygen

The natural phroperty of oil to dissolve 10% air by volume, the heat produced by the core of transformers and the catalytic effect of copper, as well as the peculiar electronic properties of the oxygen molecule trigger the well-known auto-oxidation process [SI: R H +0 2 > ROOH The split of the weak peroxidic bond generates two free radicals of unequal size. ROOH hv RO. + .OH The combination of the component having the large molecular weight with a similar one gives rise to dark colour sludge. Thus, under the attack of oxygen, both soluble and insoluble decay products are generated. To avoid the damage caused by the chemical energy of oxygen molecules, of which paramagnetic nature is also ignored, most power transformers in the US are sealed. Although this is a cost-effective, preventive maintenance measure, the large majority of the transformers in the rest of the world are free breathing. In order to minimize the attack of oxygen on the vulnerable hydrocarbons, oxidation inhibitors are used to retard the process. The effectiveness of this solution is limited because the inhibitors cannot block the reaction between the free radicals generated by the electrical stress.

2.1.1 The Impact of Electrical Stress

The energy required for the breakdown of a sigma covalent bond is approximately 4 eV. E.O. Forster [5] described the mechanism by which the high voltage field interacts with the chemistry of insulating oils. His extensive research in this field reveals that the hidden source of energy capable of splitting covalent bonds is to be found in the electrons that escape from the conduction band and leave the surface of the metal conductor, especially during very short but frequent commutation voltage surges. The collision of these free electrons with the liquid insulation, is inevitably followed by the electronic excitation of hydrocarbon molecules [ 6 ] .While a stable molecule that reaches its singlet excitation level usually releases the absorbed energy as a quanta of light, M*>M+hv a vulnerable molecule might decompose homolitically, generating a pair of free radicals.

2.2 The Precursors of Decay Products

Due to persistent endeavours by manufacturers to enhance the quality of mineral insulating oils, their oxidation stability and gassing tendency under electrical stress have been significantly improved [9]. However, economic factors, as well the limitations of laboratory endurance tests, hinder the complete elimination of all unstable components. Consequently, most brands of new insulating oils contain small amounts of unstable hydrocarbons at delivery. As in a chemical reactor, this unknown amount of vulnerable components is gradually transformed into various decay products under the impact of heat, electrical stress, the content in dissolved oxygen and the catalytic effect of copper. Regrettably, these trace impurities have a detrimental effect on the solid insulation. According to a French researcher [lo], a selfsustaining process may cause the formation of hot spots. Therefore, a quantitative relationship should exist between the results of laboratory stability tests, and the performance of oil in service conditions. This is the objective of the newly developed testing procedures

R : H ~ > R . + .H
The fact that the molecular weight of these two fractions diflers by one or two orders of magnitude is very unilaterally interpreted. A major importance is attributed to the small fraction that, based upon Henrys Law, has the tendency to diffuse into the gas space above the surface of the oil, very little attention is given, on the other hand, to the large fraction which remains in the oil. The random chemical reactions between these short-lived intermediaries are the source of a large variety of decay products that have far-reaching effects on the development of incipient electrical failures [7]. The experimental section will provide data in support of this statement.

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described in the next section.

2.3 The Decay Products

As previously mentioned, the transformation of vulnerable hydrocarbons in decay products is a two-step process. In the first stage, the unstable chains are decomposed into short-lived primary decay products. Random chemical reactions between these intermediary decay products in the second stage generate the final decay products.

2.3.1 Primary Decay Products

Although the important role played by the broken hydrocarbon chains that are free radicals, in the deterioration of oil-paper insulation is often mentioned in the technical literature [ 111, very few maintenance planners consider them to be of practical importance. However, if their peculiar physical and chemical properties were taken into account, predictive maintenance procedures of liquid insulation could be more reliability centered. Among these peculiar properties are the following: All broken hydrocarbon chains, or knocked-out atoms are paramagnetic [12]. Under the strong electro-magnetic field of the core, they will therefore be inevitably attracted to the windings. In other words, the concentration of these chemically very reactive intermediaries will be higher inside the windings than the average content in the rest of the circulating oil. Therefore, the accumulation of sludge and x-waxes at certain points may, in fact, promote the formation of hot spots long before these insoluble trace impurities are detected as final decay products by the traditional analytical methods, such as IFT or TAN. None of the existing standard test methods for DGA, such as ASTM Designation D 3612 (131, nor the IEEE Guide for the Interpretation o f Gases i l Immersed Transformers, indicate Generated in O that the composition of combustible gases is determined by random chemical reactions between the primary decomposition products generated due to the gassing of oil. This forgotten fact concerning evolving gases under electrical stress might explain why, and we quote, analysis of these gases and the interpretation of their significance is at this time not a science, but an art subject to variability. The oxidation of oil in free breathing power

transformers is retarded by the use of oxidation inhibitors, ignoring the fact that the oxygen molecule is also paramagnetic. It is possible, therefore, that the oxygen concentration inside the windings may be higher than the amount determined by DGA in average oil samples taken from the bottom of the tank. DGA of certain aged insulating oils display dissolved oxygen contents far above the saturation level. A more realistic explanation of the large dissolved oxygen contents, exceeding the saturation level of approximately 20,000 PPM, interpreted as random variations, could be the paramagnetic nature of these gas molecules. In addition all primary decay products having an unpaired electron can catch a free electron

R. 3 Rthus becoming charge carriers and causing an increase in the dissipation factor of oil.

2.3.2 Final Decay Products

The random secondary chemical reactions between the different fractions of decomposed hydrocarbons, leads to the formation of final decay products. Some of them are gases that dissolve in the oil; others are liquids which also dissolve in the blend of hydrocarbons. The last category is made up of large hydrocarbon molecules that are no longer soluble in the liquid insulation. Depending upon the state of aggregation, the final decay products are outlined as follows:
0

Soluble Compounds in O i l Collisions between the small free radicals generated by the decomposition of certain hydrocarbon chains produce gases that dissolve in the oil. Based upon their composition as determined by chemical analysis, debatable information are obtained regarding the nature of electrical incipient failure (heat, partial discharge, etc.) that caused the decomposition reaction. The oxidation reactions of large free radicals also lead to soluble compounds. These change the chemical properties of aged oils (TAN, IFT) as well as their absorbance in the visible and ultraviolet range of the spectrum.

Insoluble Compounds in Oil When the large free radicals couple their unpaired electrons with another of similar size, a compound

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with a molecular weight between 500-600 arises. This size of hydrocarbon chains is no longer soluble in the blend. By coalescence, sludge is generated when oxygen is present; x-waxes are produced when it is absent. None of these insoluble suspensions of colloidal size can be detected by traditional testing procedures, but both can potentially clog the pores of paper insulation and to promote the formation of hot spots.

Symposium held in Calgary, Canada three years ago [14]. If the oil is degassed and saturated with nitrogen, the dissolved oxygen can be removed in a few days.

3.1.2 Environmentally Friendly Reclamation

Unlike the empirical removal of dissolved decay products by reclamation, a trustworthy and environmentally friendly technology has been developed. Currently, Fullers Earth can only be used once. After depletion it must be disposed of in a land fill. By using two organic solvents that are recoverable by atmospheric distillation however, the new reclamation procedure allows this mineral adsorbent to be reactivated and successfully reused many times. When the remaining oil in the adsorption tower is recovered by distillation of the first solvent, it can be further processed. Evaporation of the second solvent, used to remove the adsorbed decay products from the large active surface of the Fullers Earth, produces a very small amount of wasteapproximately 1% of the total volume of reclaimed oil which was treated by the tower. This tarry liquid residue, rich in aromatic hydrocarbons, can be used as feedstock by the chemical industry. A sketch of reactivation equipment is shown in a Research Report for the Canadian Electrical Association [ 151. The concept of attaching a small adsorption tower to the tank of a power transformer and continuously removing the decay products of oil in a closed loop would permit on-line reclamation of liquid insulation. When the adsorbent is depleted, the adsorption tower could be replaced by a new
one and reactivated in a central workshop. A pilot plant

3. Experimental
In order to avoid the oxidation decay of oil-paper insulation and to reduce the gassing of oil, several new techniques have been developed during recent years. Some of them consist of industrial procedures, aimed at eliminating the cause of these deficiencies. Others are state of the art testing procedures, capable of determining the effectiveness of the above-mentioned preventive maintenance technologies.

3.1 Preventive Industrial Technologies

From our perspective, the dissolved oxygen is incompatible with the dielectrical properties of liquid insulation and therefore, as the very cause of oil oxidation, it must be eliminated. Since the irreversible deterioration of paper insulation due to the gradual ageing of the oil is also harmful, the initial purity of oil should be maintained for the entire lifetime of a power transformer.

3.1.I Oxygen-Free Liquid Insulation

Based upon Henrys law, equilibrium exists between the partial pressure of gasses above the surface of oil in a power transformer and the dissolved gases in the liquid insulation. By constantly purging the gas space in an expansion chamber with a small flow of pure nitrogen at atmospheric pressure, all other dissolved gases in the oil will slowly diffuse into the inert gas above the oil. Thus, a free breathing transformer can be transformed into a sealed unit by attaching to it a small membrane nitrogen generator. An industrial experiment has shown that the oxygen content of oil in the tank of such a transformer drops from 25,000 PPM to 1,500 PPM in six months. When the amount of oxygen decreases, the rest of the dissolved gases exhibit a significantly different chemical composition. More detailed experimental data are provided in a research report presented at a Technology

constructed by the Southern Alberta Institute of Technology (SAIT) provided the opportunity to verify the effectiveness of this technology under quasi-industrial conditions.

3.2

New Testing Procedures

As long as existing testing procedures cannot establish a quantitative relationship between the purity of oil on the one hand, and the service reliability of power transformers on the other, the reclamation of aged oils is economically difficult to justify. Therefore more relevant analytical methods have been developed.

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3.2.1 Electro-Chemical Stability

The diagnosis of electrical incipient failures in power transformers by dissolved gas analysis (DGA) pays little or no attention to the gassing tendency of oil under normal operating conditions. This shortcoming, attributed to the limitations of ASTM Designation D 2300, motivated the development of an alternative stability test approved by ASTM in 1997 as Designation D 6 180 [161. This new test method measures the amount of gas generated by the oil sample subjected to electrical discharge under standard conditions by determining the increase of pressure inside the discharge cell. It also measures the increase in the dissipation factor of the oil, due to the growing number of large free radicals that catch a free electron during the five-hour test, thus becoming charge carriers.
Oil Type Dissipation Factor at 1OOoC

oxidation compounds are responsible for this shift has been confirmed by the analysis of two oil samples during the oxidation stability test. As illustrated by Fig. 1, the absorbance curve of a high stability oil submitted to the seven-day Oxidation Test D 2440 shows little change. By contrast, the low-stability oil in Fig. 2 shifts significantly during the first three days. Although no specific peak at a certain wavelength is available to characterize the ageing extent of oil in service conditions, quantification is possible by integration of the surface below the absorbance curves. Thus, the deterioration of oil purity in power transformers can be monitored on a step-by-step basis, even during the early stages of the oxidation process. An example is given in Fig. 3
Absorbance in the Visible Range of Spectrum
118

10

08

New

Samole No. 2 Sample No. 3

0.32 0.83

0.94

A O6
04

3.36

TABLE 1 Dissipation Factor Increase of Oils Subjected to an Electrical Discharge. The benefits of this new stability test are described in the Special Technical Publication STP 1376, published by ASTM last year in March [171. According to our findings, the gassing of liquid insulation is dependent not only upon the chemical composition of the hydrocarbon blend, but also on its degree of purity. In other words, the gas evolvement of an aged oil decreases after its purification by reclamation. Thus, other new testing procedures proved to be necessary to reliably assess the degree of trace impurities in aged insulating oils.

02

0 03
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nm

Fig. 1: Absorbance Curves over 7-day Oxidation Test of Good Stability New Oil

Absorbance in the Visible Range of Spectrum

~ o o
25

2o

'5 10

3.2.2 Assessment of Dissolved Impurities

Since the gassing of oil increases with the growing amount of dissolved decay products long before the IFT and TAN become reasons for concern, the spectral analysis has been found appropriate to accurately monitor the purity degree of liquid insulation. In contrast with the low absorbance shown by all brands of new oil in the visible spectrum between 360 and 600 nm, the samples taken from transformers in service usually show a shift of the absorbance curve to longer wavelengths. The assumption that the variable amounts of intermediary
05

Oo03600

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Fig. 2: Absorbance Curves over 7-day Oxidation Test of Poor StabilityNew Oil

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Absorbance in the Visible Range of Spectrum

2 00
18
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14 12
A

lo
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nrn

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DF=Dissipation Factor, T=Turbidity. ABS=Absorbance Fig. 3: Absorbance Curves of New, Slightly Oxidized and Heavily Oxidized Oils

Another advantage of this fast, inexpensive and relevant analysis lies in the fact that during the reclamation of aged oils the absorbance curve shifts in the opposite direction towards shorter wavelengths. Consequently, the effectiveness of reclamation can be objectively determined. Moreover, a cross examination of the purity of oil and its gassing pattern can be carried out. This new testing procedure is currently under ASTM Technical Committee D 27 consideration, with good chances of approval in the foreseeable future [181.

(ESZ) principle and permitted a direct measurement by counting and sizing particles smaller than 50 nm from less than 50,00O/ml in new products to tens of millions in aged transformer oil. Unlike the turbidity assessment, which is more appropriate for field routine determinations, particle counting and sizing is recommended for laboratory analysis and cross examination with DGA results. When the gas content of oil is alarming, the number of insoluble particles should also be high. In such situations it must be determined whether a low electro-chemical stability of oil, or an incipient electrical failure is the source of the particle content and gas of concern forming these decay products. Without knowing the gassing pattern of the liquid insulation under electrical stress, the DGA results alone can be very misleading. By recording the distribution curves of a new oil before and after the Stability Test D 6180 as shown in Fig. 4, the direct relationship between the gas evolvement of oil under electrical discharge and the formation of insoluble suspensions is irrefutably demonstrated and accurately determined.
lW*ld
DiffermtialNumber (Average) -New OilBefore UeclncalStaWyD 6180 (188 arO/mL) New O d ARmElect~icalShb~y D 6180(1 066 COO/$

3.2.2 Assessment of Insoluble Impurities

As mentioned above, the gassing of oil under electrical stress generates large fractions of the broken hydrocarbon chains as well as gasses. It is obvious that these chemically very reactive components are very likely to collide and couple their unpaired electron with a similar species. The end product is a large molecule that is no longer soluble in the blend of hydrocarbons. The first experimental proof that this theoretical assumption is correct has been provided by the increase of turbidity after undergoing the procedures of Stability Test D 6 180. The turbidity of insulating oil is another testing procedure developed in co-operation with the HACH Company in Loveland, CO and approved by ASTM in 1997 as Designation D 6 18 1 . [ 191. The assessment of turbidity is a quasi-quantitative determination. Therefore, another successful co-operative venture with Beckman Coulter Inc. located in Miami FA, allowed for a more accurate determination of the characteristics of insoluble suspension in new, aged, reconditioned and reclaimed oils. The state-of-the-art instrument used was based upon the electric sensing zone

6 7 8

IO

Pmiicls D~mekm(p)

Fig. 4: Particle Distribution Curve of New Oil Before and After Stability D 6180

Comparing the distribution curve of particles in a new oil and an aged oil as shown in Fig. 5, the contrast is even more striking.

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Differential Number (Average)

-AgedO~l(163mOMllmL)
410*103

-NewOd(l8

7S7Ida

5 m*103
loa*ld 0

2 i

.
3

.
4

5 i j 6 i 1 i 8 o 10 i Patticle Eameter(pxn)

20

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40 50 60

Fig.5: Comparison of Particle Distribution of New and Aged oils

Following the development of this laboratory technique for counting and sizing insoluble decay products in mineral insulating oils, a standard test method has been drafter and forwarded to ASTh4 [20]. The benefits of this new method are currently under scrutiny by the members of Technical Committee D 27. Modernisation of the analytical procedures related to the properties of liquid insulation is expected to better establish the relation between its purity and the service reliability of power transformers. With the availability of the methods necessary to establish a quantitative relationship between the results of laboratory endurance tests on one hand, and the performance of oil in real life conditions on the other, the preventive maintenance of liquid insulation will become cost effective. Moreover, environmentally friendly on-line reclamation will extend the life expectancy of the oil (a non-renewable resource), while enhancing the service reliability of power transformers.

4. Conclusions
4.1 Modernisation of the analytical techniques used in examining liquid insulation has highlighted the reality of the irreversibly damaging efSect of the deterioration of its purity on the solid insulation, and implicitly, on the service reliability of power transformers. 4.2 Taking into account all the properties of dissolved Of which is so Oxygen, the to the Purity Of Oil, it is obvious that

oxidation inhibitors cannot properly protect solid insulation against its destructive effect. 4.3 Since both the ever-present high voltage field, and dissolved oxygen can transform the small amount of precursors in decay products, the stability of oil can be maximised by minimising the content of vulnerable hydrocarbons. 4.4 Prior to becoming decay products, all components of the hydrocarbon blend in power transformers are very similar. The elimination of those that are vulnerable at the manufacturing stage is very difficult. Only the end-users have the privilege of using reclamation to selectively remove what is by then identified by a different chemical composition. 4.5 By using means now available to measure and compare the stability of insulating oils under electrical discharge, the impact of reclamation on the quality of recycled aged oil can be reliably determined. 4.6 Without measuring the gassing pattern of aged oils, the transformer fault diagnosis is based solely upon DGA, which can be very misleading. 4.7 The currently available method for determination of oil stability under laboratory conditions can generate all the decay products which arise under electrical discharge in standard conditions, namely, gases, free and x-waxes. radicals, charge

Acknowledgement
The applied research project enabling the of this paper is the result of international co-operation bemeen the private sector and educational institutions.

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Without the provision of the laboratory instruments provided by the HACH Company, Perkin-Elmer (Canada) inc. and Beckman Coulter, Inc. the results cited and conclusions reached would not have been possible. Consideration of our joint endeavours by the American Society for Testing and Materials (ASTM) and ATCO Electric Shearness Generating Station, is also gratefully acknowledged. Special thanks are due for the support received from Hilary Inyang, Ph.D., Duke Energy Distinguished Professor of Environmental Engineering at the University of North Carolina, Charlotte, NC and Director of the Global Institute for Energy and Environmental Systems (GIEES).

References

1 Darwenzia, M., Hill, D., Tri Le and Saha, T.K., Studies o f the Condition o f Insulation in Aged Power Transformers, Part 2, Fundamental Electrical and Chemical Considerations, Proceedings of the 3rd International Conference of Properties and Applications of Dielectric Materials, July 18-20, 1989, Tokyo, Japan.
2 Designation D 2440-99, Standard Test Method for Oxidation Stability of Mineral Insulating Oil, Vol. 10.03. IEEE Guide for the Interpretation o f Gases 3 Generated in Oil Immersed Transformers, IEEE Std. C57.104- 1991. 4 Sabau, J. and Stokhuyzen, R., Aging and Gassing of Mineral Insulating Oils, Proceedings of TechCon 2000, Dave Hanson, Editor, TJ/J2b, Sacramento, CA. Forster, E.O. Electrical Breakdown of Dielectric 5 Fluids, ASTM Monograph 2, Engineering Dielectrics, Vol. 111, chapter 3, January 1994.

6 Mousseron-Canet, M. and Mani, J.C., Photochemistry and Molecular Reactions, Dunod, Paris, 1969.
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Transformers, Proceedings of SAIT/CEA Technology

Symposium, Calgary, AB, June 1997.

8 Fossey, J., Lefort, D. and Serba, J., Free Radicals in Organic Chemistry, John Wiley & Sons, Masson, 1995.

9 ASTM Designation D 2300-00, Standard Test Method for Gassing of Insulation Oils Under Electrical Stress and Ionization (Modified Pirelli Method), Vol. 10.03. 10 Christian Mayoux, On the Degradation of Insulating Materials Withstanding Electrical Stress, IEEE Transactions on Dielectrics and Electrical Insulation, Vol. 7, pp. 59-60, October, 2000.

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11 Tanaka, J., Free Radicals in Electrical Insulation, Proceedings of the Nineteenth Symposium on Electrical Insulating Materials, Osaka, Japan, 1986. 12 Pryor, W.W., Free Radicals, Inc., New York, 1966. McGraw-Hill,

13 ASTM Designation D 3612, Standard Test Method for Analysis of Gases Dissolved in Electrical Insulating Oil by Gas Chromatography, Vol. 10.03. 14 Sabau, J., A New Type of Nitrogen Blanketing System for Freely Breathing Power Transformers. Report prepared by INSOIL Canada Ltd. for the Southern Alberta Institute of Technology (SAIT), June 1998, Calgary, AB., Canada. 15 Sabau, J., Purification of Aged Insulating Oils by Regenerable Resin, Part B, Report 334 T 768A, prepared by INSOIL Canada Ltd., for the Canadian Electrical Association, April, 1994, Pontreal PQ, Canada. 16 ASTM Designation D 6180-97, Standard Test Method for Stability of Insulating Oils of Petroleum Origin Under Electrical Discharge, Vol. 10.3. 17 Sabau, J. and Stokhuyzen, R., Electrochemical Stability of Mineral Insulating Oils, ASTM, STP 1376, Electrical Insulating Materials, International, Issues, Marcel M. Hirscheler, Ed., March 2000.

18 Standard Test Method for Determination of the Relative Content of Dissolved Decay Products in Mineral Insulating Oils by Spectrophotometry, (Under consideration by ASTM).
19 ASTM Designation D 6181-97, Standard Test Method for Measurement of Turbidity in Mineral Insulating Oil of Petroleum Origin, Vol. 10.3. 20 Standard Test Method for Determining the Size and Number of Particles in Mineral Insulating Oills of Petroleum Origin Using the Electric Sensing Zone (ESZ) Principle. (Under consideration by ASTM).

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