ASTM D1698-03(2008)
(Test Method)Standard Test Method for Sediments and Soluble Sludge in Service-Aged Insulating Oils (Withdrawn 2014)
Standard Test Method for Sediments and Soluble Sludge in Service-Aged Insulating Oils (Withdrawn 2014)
SIGNIFICANCE AND USE
Sediment in insulating oil may deposit on transformer parts and interfere with heat transfer and may choke oil ducts; thus hindering oil circulation and heat dissipation. Inorganic sediment usually indicates contamination of some type and organic sediment indicates either deterioration of the oil or contamination.
Soluble sludge indicates deterioration of the oil, presence of contaminants, or both. It serves as a warning that formation of sediment may be imminent.
The determination of sediment and soluble sludge in a used insulating oil assists in deciding whether the oil may continue to be used in its existing condition or should be replaced, reclaimed, or reconditioned.
SCOPE
1.1 This test method covers the determination of sediment and soluble sludge in service-aged insulating oils of petroleum origin. Also, provision is made for determining organic and inorganic content of the sediment. The method is intended primarily for oils of comparatively low viscosity; for example 5.7 to 13.0 cSt (mm2/s) at 40°C (104°F). Suitability for high viscosity oils have not been determined.
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 may involve hazardous materials, operations, and equipment. 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 and health practices and determine the applicability of regulatory limitations prior to use.
WITHDRAWN RATIONALE
This test method covers the determination of sediment and soluble sludge in service-aged insulating oils of petroleum origin.
Formerly under the jurisdiction of Committee D27 on Electrical Insulating Liquids and Gases, this test method was withdrawn in May 2014. This standard is being balloted for withdrawal with no replacement because it is no longer used within the industry.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D1698 − 03(Reapproved 2008)
Standard Test Method for
Sediments and Soluble Sludge in Service-Aged Insulating
Oils
This standard is issued under the fixed designation D1698; 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 and that can be separated by centrifuging under certain
prescribed conditions.
1.1 This test method covers the determination of sediment
3.1.4 soluble sludge—oil deterioration products or
and soluble sludge in service-aged insulating oils of petroleum
contaminants, or both, which become insoluble upon dilution
origin. Also, provision is made for determining organic and
with n-pentane under prescribed conditions.
inorganic content of the sediment. The method is intended
primarily for oils of comparatively low viscosity; for example
4. Summary of Test Method
5.7 to 13.0 cSt (mm /s) at 40°C (104°F). Suitability for high
viscosity oils have not been determined.
4.1 A sample portion is centrifuged to separate sediment
from the oil. The upper, sediment-free portion is decanted and
1.2 The values stated in SI units are to be regarded as
retained for determination of soluble sludge. The sediment is
standard. No other units of measurement are included in this
dislodged and filtered through a filtering crucible.After drying
standard.
and weighing to obtain total sediment the crucible is ignited at
1.3 This standard may involve hazardous materials,
500°C and reweighed. Loss in weight is organic and the
operations, and equipment. This standard does not purport to
remainder is inorganic content of sediment. Soluble sludge is
address all of the safety concerns, if any, associated with its
determined on the sediment-free portion by dilution with
use. It is the responsibility of the user of this standard to
n-pentane to precipitate n-pentane insolubles, and filtration
establish appropriate safety and health practices and deter-
through a filtering crucible or 0.45 µm filter membrane.
mine the applicability of regulatory limitations prior to use.
5. Significance and Use
2. Referenced Documents
5.1 Sediment in insulating oil may deposit on transformer
2.1 ASTM Standards:
parts and interfere with heat transfer and may choke oil ducts;
D923 Practices for Sampling Electrical Insulating Liquids
thus hindering oil circulation and heat dissipation. Inorganic
D2440 Test Method for Oxidation Stability of Mineral
sediment usually indicates contamination of some type and
Insulating Oil
organic sediment indicates either deterioration of the oil or
3. Terminology contamination.
3.1 Definitions of Terms Specific to This Standard: 5.2 Soluble sludge indicates deterioration of the oil, pres-
3.1.1 inorganic sediment—that portion of the total sediment ence of contaminants, or both. It serves as a warning that
which remains after ignition at 500°C. formation of sediment may be imminent.
3.1.2 organic sediment—that portion of the total sediment
5.3 The determination of sediment and soluble sludge in a
which is lost during ignition at 500°C.
used insulating oil assists in deciding whether the oil may
continue to be used in its existing condition or should be
3.1.3 sediment—any solid substance or substances that are
replaced, reclaimed, or reconditioned.
insoluble in the oil under test at ordinary room temperatures,
6. Apparatus
This test method is under the jurisdiction of ASTM Committee D27 on
6.1 Centrifuge Tube, 30-mLcapacity, preferably with round
Electrical Insulating Liquids and Gasesand is the direct responsibility of Subcom-
mittee D27.07 on Physical Test.
or elliptical bottom to facilitate removal of sediment. Pear-
Current edition approved May 1, 2008. Published June 2008. Originally
shaped tubes are not recommended.
approved in 1959. Last previous edition approved in 2003 as D1698 – 03. DOI:
10.1520/D1698-03R08.
6.2 Centrifuge, capable of whirling two or more filled
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
centrifuge tubes at a speed which can be controlled to give a
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
relative centrifugal force (rcf) between 600 and 700 at the tips
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. of the tubes. The revolving head, trunnion rings, and trunnion
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D1698 − 03 (2008)
cups, including the rubber cushion, shall be soundly con- using n-pentane as the washing agent. Make certain that any
structedtowithstandthemaximumcentrifugalforcecapableof sediment adhering to instruments used in cleaning the tube is
being delivered by the power source. The trunnion cups and also transferred to the filtering crucible.Afilter membrane may
cushions shall firmly support the tubes when the centrifuge is be used instead of the filtering crucible if only total sediment is
inmotion.Thecentrifugeshallbeenclosedbyametalshieldor to be determined.
case strong enough to eliminate danger if any breakage occurs.
9.4 Wash the sediment in the filtering crucible thoroughly
Calculate the speed of the rotating head by means of the
with n-pentane to remove all traces of oil. Normally, three
following equation:
washes of 25-mL portions each are sufficient. A drop of the
final n-pentane washing should show no oil stain on a filter
rpm 5 265 =rcf/d
paper.
9.5 Dry the sediment in the filtering crucible by suction, and
where:
place in an oven at 105°C for drying to constant weight. Cool
rcf = relative centrifugal force, and
in a desiccator and weigh to the nearest 0.0001 g.
d = diameter of swing, in., measured between tips of
opposite tubes when in rotating position,
10. Procedure for Organic and Inorganic Sediment
or:
10.1 Wash the sediment in the filtering crucible with chlo-
roform or acetone until it is free of chloroform or acetone-
d = diameter of swing cm/2.54, measured between tips of
soluble material (see Note). Three washes of 25-mL portions
opposite tubes when in rotating position.
each are usually sufficient.
6.3 Electric Muffle Furnace, capable of maintaining a tem-
10.2 Dry the sediment by suction and ignite in the crucible
peratu
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