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ASTM D2225-04

(Test Method)

Standard Test Methods for Silicone Fluids Used for Electrical Insulation

Standard Test Methods for Silicone Fluids Used for Electrical Insulation

SIGNIFICANCE AND USE
Tests covered in this standard may be used for quality control and design considerations.
Included in each test method is a brief statement describing its significance.
SCOPE
1.1 These test methods cover the testing of silicone fluids for use in transformers, capacitors, and electronic assemblies as an insulating or cooling medium, or both. These methods are generally suitable for specification acceptance, factory control, referee testing, and research.
1.2 Although some of the test methods listed here apply primarily to petroleum-based fluids, they are, with minor revisions, equally applicable to silicone fluids.
1.3 Silicone fluids are used for electrical insulating purposes because of their stable properties at high and low temperatures and their relative environmental inertness.
1.4 A list of the properties and standards are as follows:  Property Measured Section ASTM Test Method Physical: Color 6 D 2129 Flash point 7 D 92 Fire point 7 D 92 Polychlorinated biphenyl 8 D 4059 content Pour point 9 D 97 Refractive index 10 D 1807 Specific gravity 11 D 1298, D 1481, D 4052 Volatility 12 D 4559 Viscosity 13 D 445, D 2161 Chemical: Neutralization number 14 D 974 Water content 15 D 1533 Electrical: Relative permittivity 16 D 924 2 Dielectric breakdown 17 D 877 3 voltage Dissipation factor 18 D 924 2 Specific resistance 19 D 1169 2 Compatibility 20 D 5282
1.5This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
30-Nov-2004
ICS
29.040.10 - Insulating oils
Technical Committee
D27 - Electrical Insulating Liquids and Gases
Drafting Committee
D27.02 - Gases and Non-Mineral Oil Liquids
Current Stage
Ref Project

Relations

Replaces
ASTM D2225-92(1997) - Standard Test Methods for Silicone Fluids Used for Electrical Insulation
Effective Date
01-Dec-2004
Referred By
ASTM D877/D877M-19 - Standard Test Method for Dielectric Breakdown Voltage of Insulating Liquids Using Disk Electrodes
Effective Date
01-Dec-2004
Referred By
ASTM D1816-12(2019) - Standard Test Method for Dielectric Breakdown Voltage of Insulating Liquids Using VDE Electrodes
Effective Date
01-Dec-2004
Referred By
ASTM D5282-05(2020) - Standard Test Methods for Compatibility of Construction Material with Silicone Fluid Used for Electrical Insulation
Effective Date
01-Dec-2004
Referred By
ASTM D4652-20 - Standard Specification for Silicone Liquid Used for Electrical Insulation
Effective Date
01-Dec-2004

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ASTM D2225-04 - Standard Test Methods for Silicone Fluids Used for Electrical InsulationASTM D2225-04 - Standard Test Methods for Silicone Fluids Used for Electrical Insulation
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ASTM D2225-04 - Standard Test Methods for Silicone Fluids Used for Electrical Insulation
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D2225 − 04
StandardTest Methods for
1
Silicone Fluids Used for Electrical Insulation
This standard is issued under the fixed designation D2225; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
4
1.1 These test methods cover the testing of silicone fluids 2.1 ASTM Standards:
foruseintransformers,capacitors,andelectronicassembliesas D92 Test Method for Flash and Fire Points by Cleveland
an insulating or cooling medium, or both. These methods are Open Cup Tester
generally suitable for specification acceptance, factory control, D97 Test Method for Pour Point of Petroleum Products
referee testing, and research. D445 Test Method for Kinematic Viscosity of Transparent
and Opaque Liquids (and Calculation of Dynamic Viscos-
1.2 Although some of the test methods listed here apply
ity)
primarily to petroleum-based fluids, they are, with minor
D877 Test Method for Dielectric Breakdown Voltage of
revisions, equally applicable to silicone fluids.
Insulating Liquids Using Disk Electrodes
1.3 Siliconefluidsareusedforelectricalinsulatingpurposes
D923 Practices for Sampling Electrical Insulating Liquids
because of their stable properties at high and low temperatures
D924 Test Method for Dissipation Factor (or Power Factor)
and their relative environmental inertness.
and Relative Permittivity (Dielectric Constant) of Electri-
cal Insulating Liquids
1.4 A list of the properties and standards are as follows:
D974 Test Method for Acid and Base Number by Color-
Property Measured Section ASTM Test Method
Physical: Indicator Titration
Color 6 D2129
D1169 Test Method for Specific Resistance (Resistivity) of
Flash point 7 D92
Electrical Insulating Liquids
Fire point 7 D92
Polychlorinated biphenyl 8 D4059
D1298 Test Method for Density, Relative Density (Specific
content
Gravity), or API Gravity of Crude Petroleum and Liquid
Pour point 9 D97
Petroleum Products by Hydrometer Method
Refractive index 10 D1807
Specific gravity 11 D1298, D1481, D4052
D1481 Test Method for Density and Relative Density (Spe-
Volatility 12 D4559
cific Gravity) of Viscous Materials by Lipkin Bicapillary
Viscosity 13 D445, D2161
Pycnometer
Chemical:
Neutralization number 14 D974
D1533 Test Method for Water in Insulating Liquids by
Water content 15 D1533
Coulometric Karl Fischer Titration
Electrical:
2
D1807 Test Methods for Refractive Index and Specific
Relative permittivity 16 D924
3
Dielectric breakdown 17 D877
Optical Dispersion of Electrical Insulating Liquids
voltage
D1816 Test Method for Dielectric Breakdown Voltage of
2
Dissipation factor 18 D924
2
Insulating Oils of Petroleum Origin Using VDE Elec-
Specific resistance 19 D1169
Compatibility 20 D5282
trodes
1.5 This standard does not purport to address all of the D2129 Test Method for Color of Clear ElectricalInsulating
safety concerns, if any, associated with its use. It is the Liquids (Platinum-Cobalt Scale)
responsibility of the user of this standard to establish appro-
D2161 Practice for Conversion of Kinematic Viscosity to
priate safety and health practices and determine the applica- Saybolt Universal Viscosity or to Saybolt Furol Viscosity
bility of regulatory limitations prior to use.
D2864 Terminology Relating to Electrical Insulating Liq-
uids and Gases
D4052 Test Method for Density, Relative Density, and API
1
These test methods are under the jurisdiction of ASTM Committee D27 on
Gravity of Liquids by Digital Density Meter
Electrical Insulating Liquids and Gasesand are the direct responsibility of Subcom-
mittee D27.02 on Gases and Non-Mineral Oil Liquids.
Current edition approved Dec. 1, 2004. Published January 2005. Originally
4
approved in 1963 as D2225 – 63 T. Last previous edition approved in 1997 as For referenced ASTM standards, visit the ASTM website, www.astm.org, or
D2225 – 92 (1997). DOI: 10.1520/D2225-04. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
Amodified cell cleaning procedure is given forTest Methods D924 and D1169. Standards volume information, refer to the standard’s Document Summary page on
3
A modified cell cleaning procedure is recommended for Test Method D877. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D2225 − 04
D4059 Test Method for Analysis of Polychlorinated Biphe- 7. Flash and Fire Points
nyls in Insulating Liquids by Gas Chromatography
7.1 Significance— The flash and fire points of a silicone
D4559 Test Method for Volatile Matter in Silicone Fluid
...

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This specification describes a high fire-point mineral oil based electrical insulating fluid, for use as a dielectric and cooling medium in new and existing power and distribution electrical apparatuses, such as transformers and switchgear. The material discussed here is miscible with other petroleum based insulating oils, and may not be miscible with electrical insulating liquids of non-petroleum origin. The insulating oils shall be compatible with typical material of construction of existing apparatus and will satisfactorily maintain its functional characteristic in its application. This specification applies only to new insulating material oil as received prior to any processing. Sampled specimens shall undergo appropriate tests, and shall conform correspondingly to specified physical (appearance upon visual examination, color in ASTM units, fire point, flash point, aniline point, interfacial tension, pour point, relative density, and kinematic viscosity), electrical (dielectric breakdown voltage, gassing tendency, and dissipation factor), and chemical (corrosion behavior against sulfur, inorganic chlorides and sulfates content, acid number, water content, oxidation stability, oxidation inhibitor content, and PCB content) property requirements.
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1.2 Less flammable insulating liquid differs from conventional mineral insulating liquid by possessing a fire-point of at least 300 °C. This property is necessary in order to comply with certain application requirements of the National Electrical Code (Article 450-23) or other agencies. The material discussed in this specification is miscible with other petroleum based insulating liquids. Mixing less flammable liquids with lower fire point hydrocarbon insulating liquids (for example, Specification D3487 mineral liquid) may result in fire points of less than 300 °C.  
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1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM D1524-15(2022)(Test Method)
Standard Test Method for Visual Examination of Used Electrical Insulating Liquids in the Field

SIGNIFICANCE AND USE
4.1 By use of this test method and Test Methods D1500 or D2129 the color and condition of a test specimen of electrical insulating liquid may be estimated during a field inspection, thus assisting in the decision as to whether or not the sample should be sent to a central laboratory for full evaluation. Cloudiness, particles of insulation, products of metal corrosion, or other undesirable suspended materials, as well as any unusual change in color may be detected.
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ABSTRACT
This guide describes methods of testing and specifications for electrical insulating oils of petroleum origin intended for use in electrical cables, transformers, oil circuit breakers, and other electrical apparatus where the oils are used as insulating, or heat transfer media, or both. This guide is classified into the following categories: sampling practices, physical tests, electrical tests, chemical tests, and specifications. The test methods shall be as follows: aniline point; coefficient of thermal expansion; color; examination; flash and fire point; interfacial tension; pour point of petroleum products; refractive index; relative density; specific heat; thermal conductivity; turbidity; viscosity; dielectric breakdown voltage; dissipation factor and relative permittivity; gassing tendency; resistivity; stability under electrical discharge; acidity; carbon-type composition; compatibility with construction material; copper content; furanic compounds; gas analysis; gas content; inorganic chlorides and sulfates; neutralization numbers; oxidation inhibitor content; oxidation stability; polychlorinated biphenyl content; sediment and soluble sludge; sulfur; water content; mineral insulating oil for electrical apparatus; and high firepoint electrical insulating oils.
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1.2 The purpose of this guide is to outline the applicability of the available test methods. Where more than one is available for measuring a given property, their relative advantages are described, along with an indication of laboratory convenience, precision, (95 % confidence limits), and applicability to specific types of electrical insulating liquids.  
1.3 This guide is classified into the following categories: Sampling Practices, Physical Tests, Electrical Tests, Chemical Tests, and Specifications. Within each test category, the test methods are listed alphabetically by property measured. A list of standards follows:    
Category  
Section  
ASTM Standard  
Sampling:  
3  
D923  
Physical Tests:  
Aniline Point  
4  
D611  
Coefficient of Thermal Ex-
pansion  
5  
D1903  
Color  
6  
D1500  
Examination: Visual Infrared  
7  
D1524, D2144, D2129  
Flash and Fire Point  
8  
D92  
Interfacial Tension  
9  
D971  
Pour Point of Petroleum
Products  
10  
D97, D5949, D5950  
Particle Count in Mineral
Insulating Oil  
11  
D6786  
Refractive Index and Specific
Optical Dispersion  
12  
D1218  
Relative Density (Specific
Gravity)  
13  
D287, D1217, D1298, D1481, D4052  
Specific Heat  
14  
D2766  
Thermal Conductivity  
15  
D2717  
Viscosity  
16  
D445, D2161, D7042  
Electrical Tests:  
Dielectric Breakdown Voltage  
17  
D877, D1816, D3300  
Dissipation Factor and Rela-
tive Permittivity (Dielectric
Constant)  
18  
D924  
Gassing Characteristic
Under Thermal Stress  
19  
D7150  
Gassing Tendency  
20  
D2300  
Resistivity  
21  
D1169  
Chemical Tests:  
Acidity, Approximate  
22  
D1534  
Carbon-Type Composition  
23  
D2140  
Compatibility with Construc-
tion Material  
24  
D3455  
Copper Content  
25  
D3635  
Elements by Inductively
Coupled Plasma (ICP-AES)  
26  
D7151  
Furanic Compounds in
Electrical Insulating Liquids  
27  
D5837  
Dissolved Gas Analysis  
28  
D3612  
Gas Content of Cable and
Capacitor Liquids  
29  
D831, D1827, D2945  
Neutralization (Acid and
Base) Numbers  
30  
D664, D974  
Oxidation Inhibitor Content  
31  
D2668, D4768  
Oxidation Stability  
32  
D1934, D2112, D2440  
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ASTM D3635-13(2021)(Test Method)
Standard Test Method for Dissolved Copper In Electrical Insulating Oil By Atomic Absorption Spectrophotometry

SIGNIFICANCE AND USE
4.1 Electrical insulating oil may contain small amounts of dissolved metals derived either directly from the base oil or from contact with metals during refining or service. When copper is present, it acts as a catalyst in promoting oxidation of the oil. This test method is useful for research for new oils and to assess the condition of service-aged oils. Consideration should be given to the limits of detection outlined in the scope.
SCOPE
1.1 This test method covers the determination of copper in new or used electrical insulating oil of petroleum origin by atomic absorption spectrophotometry.  
1.2 The lowest limit of detectability is primarily dependent upon the method of atomization, but also upon the energy source, the fuel and oxidant, and the degree of electrical expansion of the output signal. The lowest detectable concentration is usually considered to be equal to twice the maximum variation of the background. For flame atomization, the lower limit of detectability is generally in the order of 0.1 ppm or 0.1 mg/kg. For non-flame atomization, the lower limit of detectability is less than 0.01 ppm.  
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Standard Test Method for 2,6-di-tert-Butyl- p-Cresol and 2,6-di-tert-Butyl Phenol in Electrical Insulating Oil by Infrared Absorption

SIGNIFICANCE AND USE
3.1 The quantitative determination of 2,6-ditertiary-butyl paracresol and 2,6-ditertiary-butyl phenol in a new electrical insulating oil measures the amount of this material that has been added to the oil as protection against oxidation. In a used oil it measures the amount remaining after oxidation has reduced its concentration. The test is also suitable for manufacturing control and specification acceptance.  
3.2 When an infrared spectrum is obtained of an electrical insulating oil inhibited with either of these compounds there is an increase in absorbance of the spectrum at several wavelengths (or wavenumbers). 2,6 ditertiary-butyl paracresol produces pronounced increases in absorbance at 2.72 μm (3650 cm−1), and 11.63 μm (860 cm−1 ). 2,6 ditertiary-butyl phenol produces pronounced increases in absorbance at 2.72 μm (3650 cm−1) and 13.42 μm (745 cm −1).  
3.3 When making this test on other than a highly oxidized oil or when using a double-beam spectrophotometer, it has been found convenient to obtain the spectrum between 2.5 μm (4000 cm−1) and 2.9 μm (3450 cm−1) because the instrument is compensated for the presence of moisture and the band is not influenced by intermolecular forces (associations). However, when testing a highly oxidized oil or when using a single-beam instrument better results may be obtained if the scan is made between 10.90 μm (918 cm−1) and 14.00 μm (714 cm−1).  
3.4 Increased absorption at 11.63 μm (860 cm −1) or 13.42 μm (745 cm−1) or both, will identify the inhibitor as 2,6-ditertiary-butyl paracresol or 2,6-ditertiary-butyl phenol respectively (Note 1).
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SCOPE
1.1 This test method covers the determination of the weight percent of 2,6-ditertiary-butyl paracresol (DBPC) and 2,6-ditertiary-butyl phenol (DBP) in new or used electrical insulating oil in concentrations up to 0.5 % by measuring its absorbance at the specified wavelengths in the infrared spectrum.  
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ASTM D2144-07(2021)(Practice)
Standard Practices for Examination of Electrical Insulating Oils by Infrared Absorption

SIGNIFICANCE AND USE
5.1 The infrared spectrum of an electrical insulating oil is a record of the absorption of infrared energy over a range of wavelengths. The spectrum indicates the general chemical composition of the test specimen.  
Note 2: The infrared spectrum of a pure chemical compound is probably the most characteristic property of that compound. However, in the case of oils, multicomponent systems are being examined whose spectra are the sum total of all the spectra of the individual components. Because the absorption bands of the components may overlap, the spectrum of the oil is not as sharply defined as that for a single compound. For these reasons, these practices may not in every case be suitable for the quantitative estimation of the components of such a complex mixture as mineral oil.
SCOPE
1.1 These practices are to be used for the recording and interpretation of infrared absorption spectra of electrical insulating oils from 4000 cm−1 to 400 cm−1 (2.5 μm to 25 μm).  
Note 1: While these practices are specific to ratio recording or optical null double-beam dispersive spectrophotometers, single-beam and HATR (horizontal attenuated total reflectance), Fourier-transform rapid scan infrared spectrophotometers may also be used. By computerized subtraction techniques, ratio methods can be used. Any of these types of equipment may be suitable if they comply with the specifications described in Practice E932.  
1.2 Two practices are covered, a Reference Standard Practice and a Differential Practice.  
1.3 These practices are designed primarily for use as rapid continuity tests for identifying a shipment of oil from a supplier by comparing its spectrum with that obtained from previous shipments, or with the sample on which approval tests were made. They also may be used for the detection of certain types of contamination in oils, and for the identification of oils in storage or service, by comparison of the spectra of the unknown and known oils. The practices are not intended for the determination of the various constituents of an oil.  
1.4 Warning—Infrared absorption is a tool of high resolving power. Conclusions as to continuity of oil quality should not be drawn until sufficient data have been accumulated so that the shipment-to-shipment variation is clearly established, for example.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM D2440-13(2021)(Test Method)
Standard Test Method for Oxidation Stability of Mineral Insulating Oil

SIGNIFICANCE AND USE
4.1 The oxidation stability test of mineral transformer oils is a method for assessing the amount of sludge and acid products formed in a transformer oil when the oil is tested under prescribed conditions. Good oxidation stability is necessary in order to maximize the service life of the oil by minimizing the formation of sludge and acid. Oils that meet the requirements specified for this test in Specification D3487 tend to minimize electrical conduction, ensure acceptable heat transfer, and preserve system life. There is no proven correlation between performance in this test and performance in service, since the test does not model the whole insulation system (oil, paper, enamel, wire). However, the test can be used as a control test for evaluating oxidation inhibitors and to check the consistency of oxidation stability of production oils.
SCOPE
1.1 This test method determines the resistance of mineral transformer oils to oxidation under prescribed accelerated aging conditions. Oxidation stability is measured by the propensity of oils to form sludge and acid products during oxidation. This test method is applicable to new oils, both uninhibited and inhibited, but is not well defined for used or reclaimed oils.  
Note 1: A shorter duration oxidation test for evaluation of inhibited oils is available in Test Method D2112.
Note 2: For those interested in the measurement of volatile acidity, reference is made to IEC Method 61125. 2  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM D8086-20(Test Method)
Standard Test Method for Determination of Methanol and Ethanol in Electrical Insulating Liquids of Petroleum Origin by Headspace (HS)-Gas Chromatography (GC) Using Mass Spectrometry (MS) or Flame Ionization Detection (FID)

SIGNIFICANCE AND USE
5.1 Methanol and ethanol are generated by the degradation of cellulosic materials used in the solid insulation systems of electrical equipment. More particularly, methanol comes from the depolymerization of cellulosic materials.3, 4, 5, 6  
5.2 Methanol and ethanol, which are soluble in an insulating liquid to an appreciable degree, will proportionally migrate to that liquid after being produced from the cellulose.  
5.3 High concentrations or unusual increases in the concentrations of methanol or ethanol, or both, in an insulating liquid may indicate cellulose degradation from aging or incipient fault conditions. Testing for these alcohols may be used to complement dissolved gas-in-oil analysis and furanic compounds as performed in accordance with Test Methods D3612 and D5837 respectively.
SCOPE
1.1 This test method describes the determination of by-products of cellulosic materials degradation found in electrical insulation systems that are immersed in insulating liquid. Such materials include paper, pressboard, wood and cotton materials. This test method allows the analysis of methanol and ethanol from the sample matrix by headspace GC-MS or GC-FID.  
1.2 This test method has been used to test for methanol and ethanol in mineral insulating liquids and less flammable electrical insulating liquids of mineral origin as defined in D3487 and D5222 respectively. Currently, this method is not a practical application for ester liquids.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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