Standard Test Method for Volatile Matter in Silicone Fluid

SIGNIFICANCE AND USE
High values may indicate contamination of the silicone with other materials, inadequate removal of volatile components by the producer, or the presence of a depolymerization catalyst.
The outcome will be affected directly by the presence of any high vapor pressure material in the sample, such as solvents or low molecular weight silicones.
A high volatile content could also indicate the presence of a depolymerization catalyst in the fluid. The time and temperature specified in this test method are ideal for detecting the effect of such a material, as the depolymerization takes place at a highly accelerated rate and the low molecular weight components are rapidly evaporated. The result is a very significant weight loss during the test period. The exact amount depends on the type and amount of catalyst present. The conditions specified in the method should not cause measureable depolymerization of silicone if such a catalyst is not present.
SCOPE
1.1 This test method describes a procedure for determining the volatile matter in silicone fluids used for electrical insulation.
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 whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

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Publication Date
30-Apr-2010
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ASTM D4559-99(2010) - Standard Test Method for Volatile Matter in Silicone Fluid
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4559 − 99 (Reapproved 2010)
Standard Test Method for
Volatile Matter in Silicone Fluid
This standard is issued under the fixed designation D4559; 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 temperature specified in this test method are ideal for detecting
the effect of such a material, as the depolymerization takes
1.1 This test method describes a procedure for determining
place at a highly accelerated rate and the low molecular weight
the volatile matter in silicone fluids used for electrical insula-
components are rapidly evaporated. The result is a very
tion.
significantweightlossduringthetestperiod.Theexactamount
1.2 The values stated in SI units are to be regarded as
depends on the type and amount of catalyst present. The
standard. No other units of measurement are included in this
conditions specified in the method should not cause measure-
standard.
able depolymerization of silicone if such a catalyst is not
1.3 This standard does not purport to address all of the
present.
safety concerns, if any, associated with its use. It is the
5. Apparatus
responsibility of whoever uses this standard to consult and
establish appropriate safety and health practices and deter-
5.1 Air-circulating Oven, capable of meeting the require-
mine the applicability of regulatory limitations prior to use.
ments of Specification D5423.
5.2 Griffın Pyrex Beakers, 50-mL, with the following di-
2. Referenced Documents
mensions:
2.1 ASTM Standards:
5.2.1 Outside Diameter—42 6 0.6 mm.
D923 Practices for Sampling Electrical Insulating Liquids
5.2.2 Wall Thickness—0.14 to 0.165 mm.
D5423 Specification for Forced-Convection Laboratory Ov-
5.3 Analytical Balance, capable of measuring to 1 mg.
ens for Evaluation of Electrical Insulation
6. Sampling
3. Summary of Test Method
6.1 Obtain a sample of the silicone fluid to be tested using
3.1 Specimens are weighed before and after heating for a
appropriateASTM sampling apparatus in accordance withTest
specific time in a forced air oven to determine weight loss.
Methods D923.
4. Significance and Use
7. Procedure
4.1 High values may indicate contamination of the silicone
7.1 Clean two 50-mL beakers by washing in toluene,
with other materials, inadequate removal of volatile compo-
followed by a rinse in acetone or other appropriate cleaning
nents by the producer, or the presence of a depolymerization
method.
catalyst.
7.2 Bake two 50-mL beakers at 150 6 5°C for a minimum
4.2 The outcome will be affected directly by the presence of
of 1 h, transfer to a desiccator using clean, dry gloves or
any high vapor pressure material in the sample, such as
crucible tongs and cool the beakers to ambient temperatures.
solvents or low molecular weight silicones.
Use clean, dry gloves or crucible tongs to handle beakers from
4.3 A high volatile content could also indicate the presence
this point forward. Weigh each beaker to the nearest mg (T).
of a depolymerization catalyst in the fluid. The time and
7.3 Weigh a 2.0 6 0.2 g sample to the nearest mg in each
beaker (W ).
This test method is under the jurisdiction of ASTM Committee D27 on
7.4 Heat at 150 6 5°C in an air circulating oven for 24 6
Electrical Insulating Liquids and G
...

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